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. ft .-. .. , EA'A lJnited Stat~s Envi1onmental Pmtettion '' Agenc~ Region 6 Compliance Assurance and Enforcement Division INSPECTION REPORT Inspection Date(s): Media: Regulatory Program(s) October 24, 2017 Water NPDES Company Name: Facility Name: Facility Physical Location: (city, state, zip code) Mailing address: (city, state, zip code) County/Parish: Facility Contact: Exxon Mobil Chemical Company Exxon Mobil Baton Rouge Chemical Plant 4999 Scenic HWY Baton Rouge, LA 70805 +------- PO Box 241 .Baton Rouge, LA 70821 East Baton Rouge Parish David Gatz Wastewater Advisor (225) 400-1440 f.david.gatz@exxonmobil.com FRS Number: Identification/Permit Number: Media Number: NAICS: SIC: 110000449970 AI# 286 / LPDES Permit# LA0005401 325110-Petrochemical Manufacturing, 325199-0ther Basic Organic Chemical Manufacturing, 325211-Piastics Material and Resin Manufacturing, 325212Synthetic Rubber Manufacturing, 48611-Pipeline Transportation of Crude Oil, 48211-Rail Transportation, 32511-Petrochemical Manufacturing, 32521-Resin and Synthetic Rubber Manufacturing 2869-lndustrial Organic Chemicals, 2813-lndustrial Gases, 2822-Synthetic Rubber, 2865-Cyclic Crudes etc., and 4952-Sanitary Personnel participating in inspection: Rachel Matthews ---------------- Mike Tillman EPA- Region 6 EPA- Region 6 Margaret Parker LDEQ David Gatz ExxonMobil -----------------. Haley Delk ExxonMobil Joey Rinaudo ExxonMobil Life Scientist Environmental Scientist Environmental Scientist Ill Wastewater Advisor AWT Contact Engineer Environmental Regulatory Program Supervisor 214-665-8589 214-665-7531 225-219-3173 225-400-1440 225-316-9105 225-397-4623 -- --- - - EPA Lead Inspector ~I Signature/Date Matthews Supervisor - Signature/Date IC .4nf/f Wk Carol Peters-Wagnon -- . D~i~--;;;x;./?'"/;. .... (.:</!7/!7 Date 6ENFORM-019-R6 (10/6/14) 1 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Section I - INTRODUCTION PURPOSE OF THE INSPECTION EPA Region 6 inspectors Rachel Matthews and Mike Tillman arrived at the ExxonMobil Baton Rouge Chemical Plant (Plant) at 9:00am on October 24, 2017 for an unannounced Compliance Evaluation Inspection (CEI). After initial facility entry we met with David Gatz, Wastewater Advisor of the Plant, as well as other staff, at the Opening Conference. We presented our credentials to Mr. Gatz and informed him this was an EPA inspection to determine compliance with the facility's National Pollutant Discharge Elimination System (NPDES) permit and Clean Water Act (CWA). The inspection was conducted under the authority of the NPDES permit program, in accordance with the Federal CWA. This report is based on information supplied by the Plant's representatives (the permittee), observations made by the U.S. EPA inspector(s), and records and reports maintained by the permittee, the State of Louisiana, and the U.S. EPA. FACILITY DESCRIPTION The Plant is located on Scenic Hwy in Baton Rouge, East Baton Rouge Parish. It is a petrochemical processing and manufacturing facility, founded in 1940, and completely built out on 150 acres. With approximately 930 full time employees and 1000 contract employees, this facility manufactures over six (6) billion pounds of petrochemical products annually. Primary products include various organic chemicals, synthetic rubber, and petroleum resins. Products are shipped via pipeline, railway, tankers, barges, and trucks. ExxonMobil has a refinery next to the chemical plant, with some connected operations. Combined, the two have sixteen (16) major operating units, ten (10) process units are located on the chemical plant. See aerial photo 1 in the photo log (Appendix 1) for a full view of the chemical plant. In addition, a more in-depth description of the various processes can be found in the current application. See Appendix 3 for the written description within the current permit application. The current permit (Appendix 2) was effective on September 1, 2012 with the application currently being reviewed for permit renewal. The permit includes authorization to discharge treated wastewater from six (6) outfalls. Discharges are to the Monte Sano Bayou. The primary outfall (001) for treated process and sanitary wastewater is permitted to continuously discharge treated wastewater from the various treatment units (combined to make the Advanced Wastewater Treatment system), including but not limited to: process wastewater, utility wastewater, sanitary wastewater, laboratory water, etc. as well as process area storm water. Another outfall (009) is permitted as an "emergency overflow discharge of Outfall 001 wastewaters from the advanced wastewater treatment unit" when there is "extreme rainfall conditions where the total flow exceeds the combined capacity of the transfer pumps and the five detention pumps" (See permit and permit application). The permit requires the permittee to "conduct concurrent monitoring" of 001 and 009 of certain parameters and "reported as an arithmetic sum on the DMR for Outfall 001" when 009 has discharges. There are no requirements to report discharges from 009 separately. 2 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Other outfalls are permitted for non-process wastewater, cooling tower water, fire training and equipment test waters, emergency eye/shower wash waters, non-process storm water, steam condensate, as well as river and well waters. The Advanced Wastewater Treatment (AWT) system consists of: 1) Oil/water separator with grit settling chambers, 2) Surge tanks for significant amounts of process area storm water, 3) Dissolved Air Flotation (DAF) unit, 4) Cooling tower, 5) Moving Bed Biological Reactor, 6) High Oxygen Activated Sludge Unit (UNOX), 7) Clarifiers, 8) Equalization tanks where the pH is adjusted, and 9) Sludge filter press. See Appendix 4 for the Water/Wastewater Flow Diagram. Section II - OBSERVATIONS During the inspection, we first saw the separator and outfall 009 location as well as two (2) of the four (4) surge tanks. See photos 1-3 and aerial photo 1. According to staff, during heavy rain events, when the AWT cannot keep up with inflow due to significant increases in process area storm water, the surge tanks (total capacity of 14 million gallons) are used to hold the mixed wastewater until such time as the wastewater treatment system can handle the flow. 16,000 gallons per minute pumps are used to pipe the excess water to the surge tanks. However, when the surge tanks are full, and the AWT still cannot keep up with the inflow, the gate valve at 009 is manually opened to allow the overflow (bypass) of the untreated wastewater and process area storm water (before the area is submerged). The sump area is also where the samples (grab) are taken. It was explained that staff sometimes need to sandbag the sump area to keep it from being submerged while they are accessing it. The current application includes a request to relocate the sample site for outfall 009 (currently within the sump) to the Analyzer House for safety purposes. It was explained that a pump would be added to an end cap at the pipes located at 009 sump area, which would send the samples to the Analyzer House. See photos 3 and 4. Outfalls 001 and 004 discharge between the 2 surge tank areas (see photo 5 and aerial photo 3). The Analyzer House, where samples are collected and pH is continuously monitored for Outfall 001, currently, includes a redundant composite auto-sampler set up. Both auto-samplers were calibrated by an outside company in August of 2017. At the time of the inspection, both samplers showed 3 Celsius and the log sheets for both showed a consistent 2.5 Celsius. The pH meter is calibrated in-house and connected to a continuous computer monitoring system where historical reports can be run in various sequence. See example of 1 minute, 6 minute, and hourly pH readings (Appendix 5). The electronic flow meter is also located in the Analyzer house and similar reports can also be run for gallons per minute (see Appendix 6). The inspection also included the main area of most AWT units: the cooling tower, equalization tanks, primary clarifiers, the DAF unit, the UNOX unit, final clarifiers, and Parshall Flume. The Moving Bed Biological Reactor was not inspected at this time. It is located at the northeast end of the plant. Effluent from the DAF system is sent to the Moving Bed Biological Reactor, where it is then sent back to the UNOX system. The majority of the AWT units are also located at the northwest area of the facility, close to the Analyzer House. See aerial photo 3. 3 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 The onsite inspection concluded on October 24, 2017 while we awaited requested records for review at a later date so as not to encumber ExxonMobil staff another day. After receiving the records, we conducted a review, with some follow up questions. The following was noted: 1. On May 30, 2015 storm water (normally sent to the AWT) was discharged to Outfall 009 (the overflow site) due to a heavy rainfall. Grab samples were collected on May 30, 2015. While there was not enough flow to ensure enough samples for all required analyses, the Biochemical Oxygen Demand (BOD) samples were received by the laboratory outside of the 48-hour hold time according to the lab report. Samples were collected on 5/30/2015 at 18:24 while the laboratory received them on 6/3/2015 at 15:35 (4 days later). In addition, the laboratory did not receive the samples properly preserved nor were all of them in proper containers. There was no indication of an exceedance. See Appendix 7. 2. On October 25, 2015, process wastewater and storm water discharged to Outfall 009 due to a heavy rainfall. Grab samples were collected on October 25, 2015. The Biochemical Oxygen Demand (BOD) samples were received by the laboratory outside of the 48-hour hold time according to the lab report. Samples were collected on 10/25/2015 at 19:50 while the laboratory received them on 10/28/2015 at 11:50 (almost 3 days later). In addition, there was no custody seal, chain of custody does not show sample preservation, and the name of the sampler was absent from the chain of custody form. See Appendix 8. 3. Also during the October 25, 2015 overflow, grab samples were collected from Outfall 001 on October 25, 2015 in order to "conduct concurrent monitoring" with Outfall 009, as required in the permit. The Biochemical Oxygen Demand (BOD) samples were received by the laboratory outside of the 48-hour hold time according to the lab report. Samples were collected on 10/25/2015 at 19:50 while the laboratory received them on 10/28/2015 at 11:50 (almost 3 days later). In addition, there was no custody seal, chain of custody does not show sample preservation, and the name of the sampler was absent from the chain of custody form. See Appendix 8. 4. On October 26, 2015 rain continued and overflows from Outfall 009 continued. On this day, the normally required composite and grab samples were already being collected for Outfall 001 and no grab sample was taken concurrently for Outfall 009. The permit requires samples from 009 to be collected at various times when it is overflowing: flow and pH 1/day, oil & grease and Chemical Oxygen Demand (COD) 1/week, and BOD and Total Suspended Solids (TSS) 3/week. All other parameters are at 1/quarter or 1/year. 5. Several Chain of Custody reports show the lab added preservatives to samples upon receipt, many hours after the samples were collected. See Appendix 9. Section III - AREAS OF CONCERN Concern - The V-notch weirs on each of the final clarifiers were in need of maintenance, requiring cleaning. Algae blooms and other debris collecting on the weirs were causing system short circuiting. (See photo 6). The flow gauge on the Parshall Flume prior to final discharge to 001 was dirty and unreadable. (See photo 7) Requirement - The permit, under Part III, Section B 3 Proper Operation and Maintenance, requires the permittee to "properly operate and maintain all facilities and systems of treatment and control (and 4 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 related appurtenances) which are installed or used by the permittee to achieve compliance with the conditions of the permit. Proper operation and maintenance also includes adequate laboratory controls and appropriate quality assurance procedures". Concern - Multiple failures within the sample delivery methods and chain of custody as mentioned above with regard to chain of custody reviews. These include: 1. Hold times exceeded, 2. No custody seal, 3. Chain of custody does not show type of sampling container used or sample preservation, 4. Use of incorrect sampling containers, 5. The name of the sampler was absent from the chain of custody form, and 6. Preservatives not added as soon as possible after collection Requirement - The permit, under Part III, Section B 3 Proper Operation and Maintenance, requires the permittee to "properly operate and maintain all facilities and systems of treatment and control (and related appurtenances) which are installed or used by the permittee to achieve compliance with the conditions of the permit. Proper operation and maintenance also includes adequate laboratory controls and appropriate quality assurance procedures". Requirement - The permit, under Part III, Section C.5.c Monitoring Procedures, requires that "...adequate analytical quality assurance/quality control program to produce defensible data of known precision and accuracy. All quality control measures shall be assessed and evaluation on an on-going basis and quality control acceptance criteria shall be used to determine the validity of the data. All method specific quality control as prescribed in the method shall be followed..." Section IV - FOLLOW UP The following requested information was received by EPA on October 24, 2017 after the inspection Sample and monitoring analyses Chain-of-custody reports Waste manifests PDF version of facility layout PDF version of flow diagram Section V - LIST OF APPENDICES Appendix 1 - Photo Log Appendix 2 - Permit Appendix 3 - Permit Application, written description section Appendix 4 - Water/Wastewater Flow Diagram Appendix 5 - Example pH readings, screen shot Appendix 6 - Example flow meter readings, screen shot Appendix 7 - June 15, 2017 Letter and Monitoring Report Appendix 8 - November 13, 2015 Letter and Monitoring Report Appendix 9 - Multiple Chain of Custody Reports 5 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 1 Photograph Log UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Aerial Photo 1 - View of facility from Google Maps UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Photo 1 - Sump with Gate Valve to allow emergency overflow at outfall 009. When necessary, gate valve opened manually with pulley. Samples for 009 taken within sump. Photo 2 - standing on sump grate looking at location to outfall 009 on other side of wall UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Photo 3 - Piping where alternative sample point can be added for outfall 009. Two of four surge tanks in background. Photo 4 (Snip of NW corner of facility layout) location of Analyzer House and several outfalls UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Aerial Photo 2 - View of separator unit, sump and gate valve for outfall 009 at end of unit, outfall 009 location, and partial view of one surge tank, using Bing Maps. Photo 5 - Outfalls 001 and 004 discharge between the 2 surge tank areas, with view of the 2 western most tanks. UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Aerial Photo 3 - Majority of AWT Units, plus some outfall locations. Photo 6 - clarifier UNITED STATES ENVIRONMENTAL PROTECTION AGENCY Photograph Log Location: ExxonMobil Baton Rouge Chemical Plant City: Baton Rouge County/Parish: East Baton Rouge State: LA Photo 7 - Flow gauge at Parshall Flume ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 2 - Permit 6 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 3 - Permit Application, written description section 7 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 4 - Water/Wastewater Flow Diagram 8 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 5 - Example pH readings, screen shot 9 Appendix 5 - Example pH readings, screen shot ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 6 - Example flow meter readings, screen shot 10 Appendix 6 - Example flow meter readings, screen shot ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 7 - June 15, 2017 Letter and Monitoring Report 11 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 8 - November 13, 2015 Letter and Monitoring Report 12 NELAP CERTIFICATE NUMBER: 01955 DOD ELAP CERTIFICATE NUMBER: L14-243 Cover ANALYTICAL RESULTS PERFORMED BY GCAL, LLC 7979 Innovation Park Dr. Baton Rouge, LA 70820 Report Date 11/11/2015 GCAL Report 215102816 9999999999 Project BR Chemical Plant Deliver To Momin Birjis ExxonMobil Chemical PO Box 551 Baton Rouge, LA 70821 Additional Recipients NONE GCAL Report#: 215102816 Page 1 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Laboratory Endorsement Sample analysis was performed in accordance with approved methodologies provided by the Environmental Protection Agency or other recognized agencies. The samples and their corresponding extracts will be maintained for a period of 30 days unless otherwise arranged. Following this retention period the samples will be disposed in accordance with GCAL's Standard Operating Procedures. Common Abbreviations that may be Utilized in this Report ND DO MI TNTC SUBC FLD DL DL LOD LOQ RE 00:01 Indicates the result was Not Detected at the specified reporting limit Indicates the result was Diluted Out Indicates the result was subject to Matrix Interference Indicates the result was Too Numerous To Count Indicates the analysis was Sub-Contracted Indicates the analysis was performed in the Field Detection Limit Diluted analysis - when appended to Client Sample ID Limit of Detection Limit of Quantitation Re-analysis Reported as a time equivalent to 12:00 AM Reporting Flags that may be Utilized in this Report J or I J U B or V Q * E E Indicates the result is between the MDL and LOQ DOD flag on analyte in the parent sample for MS/MSD outside acceptance criteria Indicates the compound was analyzed for but not detected Indicates the analyte was detected in the associated Method Blank Indicates a non-compliant QC Result (See Q Flag Application Report) Indicates a non-compliant or not applicable QC recovery or RPD - see narrative The result is estimated because it exceeded the instrument calibration range Metals - % diference for the serial dilution is > 10% Sample receipt at GCAL is documented through the attached chain of custody. In accordance with NELAC, this report shall be reproduced only in full and with the written permission of GCAL. The results contained within this report relate only to the samples reported. The documented results are presented within this report. This report pertains only to the samples listed in the Report Sample Summary and should be retained as a permanent record thereof. The results contained within this report are intended for the use of the client. Any unauthorized use of the information contained in this report is prohibited. I certify that this data package is in compliance with the NELAC Institute standard and terms and conditions of the contract and Statement of Work both technically and for completeness, for other than the conditions in the case narrative. Release of the data contained in this hardcopy data package and in the computer readable data submitted has been authorized by the Quality Assurance Manager or his/her designee, as verified by the following signature. Estimated uncertainty of measurement is available upon request. This report is in compliance with the DOD QSM as specified in the contract if applicable. Authorized Signature GCAL Report 215102816 GCAL Report#: 215102816 Page 2 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Certifications 10/02/2015 Certification DOD ELAP Alabama Arizona Arkansas Colorado Delaware Florida Georgia Hawaii Idaho Illinois Indiana Kansas Kentucky Louisiana Maryland Massachusetts Michigan Mississippi Missouri Montana Nebraska New Mexico North Carolina North Dakota Oklahoma South Carolina South Dakota Tennessee Texas Vermont Virginia USDA Soil Permit Certification Number L14-243 01955 AZ0718 12-060-0 01955 01955 E87854 01955 01955 01955 200048 01955 E-10354 95 01955 01955 01955 01955 01955 01955 N/A 01955 01955 618 R-195 9403 73006001 01955 01955 T104704178 01955 460215 P330-10-00117 GCAL Report#: 215102816 Page 3 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Case Narrative Client: ExxonMobil Chemical Report: 215102816 Gulf Coast Analytical Laboratories received and analyzed the sample(s) listed on the Report Sample Summary page of this report. Receipt of the sample(s) is documented by the attached chain of custody. This applies only to the sample(s) listed in this report. No sample integrity or quality control exceptions were identified unless noted below. VOLATILES MASS SPECTROMETRY In the EPA 624 analysis, sample 21510281601 (SEPARATOR OUTFALL 009) had to be diluted due to the presence of non-target background. This dilution is reflected in the elevated reporting limits. SEMI-VOLATILES MASS SPECTROMETRY In the EPA 625 analysis, sample 21510281601 (SEPARATOR OUTFALL 009) had to be diluted to bracket the concentration of target compounds within the calibration range of the instrument and to eliminate interference from non-target background. This is reflected in elevated reporting limits. The recoveries for the surrogates are not applicable for those analyses at a 10 or higher dilution. In the EPA 625 analysis, sample 21510281602 (UNOX EFFLUENT OUTFALL 001) had to be diluted to eliminate interference from non-target background. This is reflected in elevated detection limits. METALS In the EPA 200.8 analysis for prep batch 571482, the MS/MSD recoveries and RPD are not applicable for Sodium and Vanadium because the sample concentration is greater than four times the spike concentration. The MS and/or MSD recovery is outside the control limits for Aluminum, Barium, Calcium, Manganese, Strontium, and Zirconium. The LCS recovery is within the control limits. This indicates the analysis is in control and the sample is affected by matrix interference. In the EPA 200.8 analysis for prep batch 571171, the MS/MSD recoveries and RPD are not applicable for Sodium because the sample concentration is greater than four times the spike concentration. In the EPA 200.8 analysis, samples 21510281601 (SEPARATOR OUTFALL 009) and 21510281602 (UNOX EFFLUENT OUTFALL 001) had to be diluted in order to bracket the concentration within the calibration range of the instrument. CONVENTIONALS In the BOD analysis, samples 21510281601 (SEPARATOR OUTFALL 009) and 21510281602 (UNOX EFFLUENT OUTFALL 001) were received outside of holding time. The client was notified and authorized the lab to proceed with the analysis. GCAL Report#: 215102816 Page 4 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 In the BOD analysis for sample 21510281601 (SEPARATOR OUTFALL 009), four dilutions were set up, and all were depleted of Oxygen. The corresponding greater than result is calculated using a final Dissolved Oxygen of 1.0 on the dilution using the least volume of sample. In the HACH 8000 analysis, samples 21510281601 (SEPARATOR OUTFALL 009) and 21510281602 (UNOX EFFLUENT OUTFALL 001) had to be diluted in order to bracket the concentration within the calibration range of the instrument. GCAL Report#: 215102816 Page 5 of 27 GCAL ID 21510281601 21510281602 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Summary Client ID SEPARATOR OUTFALL 009 UNOX EFFLUENT OUTFALL 001 Matrix Water Water Collect Date/Time 10/25/2015 19:50 10/25/2015 19:50 Receive Date/Time 10/28/2015 11:50 10/28/2015 11:50 GCAL Report#: 215102816 Page 6 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Detect Summary Summary of Compounds Detected SEPARATOR OUTFALL 009 SEPARATOR OUTFALL 009 EPA 624 EPA 624 CAS# 71-43-2 100-41-4 108-88-3 Parameter Benzene Ethylbenzene Toluene Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281601 Water Result 11.8 146 228 LOQ 5.00 5.00 5.00 Units ug/L ug/L ug/L EPA 625 EPA 625 CAS# 83-32-9 208-96-8 86-73-7 91-20-3 85-01-8 108-95-2 Parameter Acenaphthene Acenaphthylene Fluorene Naphthalene Phenanthrene Phenol Result 36.8 40.0 17.1 4070 31.9 42.8 LOQ 10 10 10 1000 10 10 Units ug/L ug/L ug/L ug/L ug/L ug/L EPA 200.8 EPA 200.8 CAS# 7429-90-5 7440-38-2 7440-39-3 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7440-23-5 7440-24-6 7440-32-6 7440-62-2 7440-66-6 Parameter Aluminum Arsenic Barium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Sodium Strontium Titanium Vanadium Zinc Result 4000 1.13 38.8 10100 3.55 16.7 13.5 729 14.6 1140 32.7 2.02 14.4 602 59800 82.4 13.1 483 444 LOQ 25.0 1.00 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1000 1.00 1.00 10.0 20.0 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L GCAL Report#: 215102816 Page 7 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Summary of Compounds Detected SEPARATOR OUTFALL 009 EPA 1664A EPA 1664A CAS# C-007 Parameter Oil and Grease Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 HACH 8000 HACH 8000 CAS# C-004 Parameter COD SM 2540 D-2011 SM 2540 D-2011 CAS# C-009 Parameter Total Suspended Solids UNOX EFFLUENT OUTFALL 001 UNOX EFFLUENT OUTFALL 001 EPA 625 Collect Date Receive Date EPA 625 CAS# 105-67-9 Parameter 2,4-Dimethylphenol 10/25/2015 19:50 10/28/2015 11:50 EPA 200.8 EPA 200.8 CAS# 7429-90-5 7440-39-3 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7440-02-0 7440-09-7 7440-23-5 7440-24-6 7440-32-6 Parameter Aluminum Barium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Nickel Potassium Sodium Strontium Titanium GCAL ID Matrix 21510281601 Water Result 71.5 LOQ 2.0 Units mg/L Result 192 LOQ 10.0 Units mg/L Result 45 LOQ 5 Units mg/L GCAL ID Matrix 21510281602 Water Result 22.2 LOQ 10 Units ug/L Result 2230 23.9 5530 1.91 9.01 8.19 426 9.96 637 20.5 8.22 298 29700 43.0 6.69 LOQ 25.0 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 2.00 100 1000 1.00 1.00 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L GCAL Report#: 215102816 Page 8 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Summary of Compounds Detected UNOX EFFLUENT OUTFALL 001 EPA 200.8 (Continued) CAS# Parameter 7440-62-2 7440-66-6 Vanadium Zinc Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 EPA 1664A EPA 1664A CAS# C-007 Parameter Oil and Grease HACH 8000 HACH 8000 CAS# C-004 Parameter COD SM 2540 D-2011 SM 2540 D-2011 CAS# C-009 Parameter Total Suspended Solids SM 5210 B-2011 SM 5210 B-2011 CAS# C-002 Parameter BOD GCAL ID Matrix 21510281602 Water Result 256 274 LOQ 10.0 20.0 Units ug/L ug/L Result 2.7 LOQ 2.0 Units mg/L Result 101 LOQ 10.0 Units mg/L Result 117 LOQ 5 Units mg/L Result 111 LOQ 1 Units mg/L GCAL Report#: 215102816 Page 9 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results Sample Results SEPARATOR OUTFALL 009 SEPARATOR OUTFALL 009 EPA 624 EPA 624 Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 Prep Date NA Prep Batch NA Prep Method NA Dilution 5 Analysis Date 10/29/2015 05:20 CAS# 71-55-6 79-00-5 75-34-3 75-35-4 95-50-1 107-06-2 78-87-5 541-73-1 542-75-6 106-46-7 107-13-1 71-43-2 56-23-5 108-90-7 75-00-3 67-66-3 74-87-3 100-41-4 75-09-2 127-18-4 108-88-3 156-60-5 79-01-6 75-01-4 Parameter 1,1,1-Trichloroethane 1,1,2-Trichloroethane 1,1-Dichloroethane 1,1-Dichloroethene 1,2-Dichlorobenzene 1,2-Dichloroethane 1,2-Dichloropropane 1,3-Dichlorobenzene 1,3-Dichloropropylene 1,4-Dichlorobenzene Acrylonitrile Benzene Carbon tetrachloride Chlorobenzene Chloroethane Chloroform Chloromethane Ethylbenzene Methylene chloride Tetrachloroethene Toluene trans-1,2-Dichloroethene Trichloroethene Vinyl chloride Result ND ND ND ND ND ND ND ND ND ND ND 11.8 ND ND ND ND ND 146 ND ND 228 ND ND ND GCAL ID Matrix 21510281601 Water By LBH LOQ 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 25.0 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 Analytical Batch 571221 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L CAS# 460-00-4 1868-53-7 2037-26-5 17060-07-0 Surrogate 4-Bromofluorobenzene Dibromofluoromethane Toluene d8 1,2-Dichloroethane-d4 Conc. Spiked 150 150 150 150 Conc. Rec 154 153 143 158 Units ug/L ug/L ug/L ug/L % Recovery 103 102 95 105 Rec Limits 75 - 120 73 - 125 78 - 127 70 - 123 EPA 625 EPA 625 Prep Date 10/29/2015 07:00 CAS# 120-82-1 120-83-2 105-67-9 51-28-5 121-14-2 606-20-2 95-57-8 Prep Batch 571212 Prep Method EPA 625 Parameter 1,2,4-Trichlorobenzene 2,4-Dichlorophenol 2,4-Dimethylphenol 2,4-Dinitrophenol 2,4-Dinitrotoluene 2,6-Dinitrotoluene 2-Chlorophenol Dilution 10 Analysis Date 10/30/2015 05:36 Result ND ND ND ND ND ND ND By CEK LOQ 10 20 10 20 20 20 20 Analytical Batch 571363 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L GCAL Report#: 215102816 Page 10 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results SEPARATOR OUTFALL 009 Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 EPA 625 (Continued) Prep Date 10/29/2015 07:00 Prep Batch 571212 Prep Method EPA 625 (Continued) Dilution 10 CAS# 88-75-5 534-52-1 100-02-7 83-32-9 208-96-8 120-12-7 56-55-3 50-32-8 205-99-2 207-08-9 117-81-7 218-01-9 84-66-2 131-11-3 84-74-2 206-44-0 86-73-7 118-74-1 87-68-3 67-72-1 98-95-3 85-01-8 108-95-2 129-00-0 Parameter 2-Nitrophenol 4,6-Dinitro-2-methylphenol 4-Nitrophenol Acenaphthene Acenaphthylene Anthracene Benzo(a)anthracene Benzo(a)pyrene Benzo(b)fluoranthene Benzo(k)fluoranthene Bis(2-Ethylhexyl)phthalate Chrysene Diethyl phthalate Dimethyl phthalate Di-n-butyl phthalate Fluoranthene Fluorene Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Nitrobenzene Phenanthrene Phenol Pyrene GCAL ID Matrix 21510281601 Water Analysis Date 10/30/2015 05:36 By Analytical Batch CEK 571363 Result ND ND ND 36.8 40.0 ND ND ND ND ND ND ND ND ND ND ND 17.1 ND ND ND ND 31.9 42.8 ND LOQ 10 20 20 10 10 10 10 10 10 10 10 10 10 10 20 10 10 10 10 10 10 10 10 10 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L CAS# 4165-60-0 321-60-8 1718-51-0 4165-62-2 367-12-4 118-79-6 Surrogate Nitrobenzene-d5 2-Fluorobiphenyl Terphenyl-d14 Phenol-d5 2-Fluorophenol 2,4,6-Tribromophenol Conc. Spiked 50 50 50 100 100 100 Conc. Rec Diluted Out Diluted Out Diluted Out Diluted Out Diluted Out Diluted Out Units ug/L ug/L ug/L ug/L ug/L ug/L % Recovery 0* 0* 0* 0* 0* 0* Rec Limits 43 - 120 16 - 128 43 - 138 10 - 120 10 - 120 19 - 133 GCAL Report#: 215102816 Page 11 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results SEPARATOR OUTFALL 009 EPA 625 Prep Date 10/29/2015 07:00 Prep Batch 571212 CAS# 91-20-3 Parameter Naphthalene Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281601 Water Prep Method EPA 625 Dilution 100 Analysis Date 10/30/2015 20:46 Result 4070 By CEK LOQ 1000 Analytical Batch 571399 Units ug/L EPA 200.8 EPA 200.8 Prep Date 10/28/2015 15:15 CAS# 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-24-6 7440-28-0 7440-31-5 7440-32-6 7440-66-6 7440-67-7 Prep Batch 571171 Parameter Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Strontium Thallium Tin Titanium Zinc Zirconium Prep Method EPA 200.8 Dilution 1 Analysis Date 11/02/2015 10:02 Result ND 1.13 38.8 ND ND 10100 3.55 16.7 13.5 729 14.6 1140 32.7 2.02 14.4 602 ND ND 82.4 ND ND 13.1 444 ND By LWZ LOQ 2.00 1.00 1.00 0.50 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1.00 0.50 1.00 0.50 1.00 1.00 20.0 1.00 Analytical Batch 571497 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L EPA 200.8 Prep Date 10/28/2015 15:15 CAS# 7429-90-5 7440-23-5 Prep Batch 571171 Parameter Aluminum Sodium Prep Method EPA 200.8 Dilution 10 Analysis Date 11/02/2015 09:59 Result 4000 59800 By LWZ LOQ 25.0 1000 Analytical Batch 571497 Units ug/L ug/L GCAL Report#: 215102816 Page 12 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results SEPARATOR OUTFALL 009 Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 EPA 200.8 (Continued) Prep Date 10/28/2015 15:15 Prep Batch 571171 Prep Method EPA 200.8 (Continued) Dilution 10 CAS# 7440-62-2 Parameter Vanadium GCAL ID Matrix 21510281601 Water Analysis Date 11/02/2015 09:59 By Analytical Batch LWZ 571497 Result 483 LOQ 10.0 Units ug/L EPA 245.2 EPA 245.2 Prep Date 11/02/2015 09:45 CAS# 7439-97-6 Prep Batch 571481 Parameter Mercury Prep Method EPA 245.2 Dilution 1 Analysis Date 11/02/2015 14:13 Result ND By LWZ LOQ 0.00020 Analytical Batch 571521 Units mg/L EPA 1664A EPA 1664A Prep Date 10/29/2015 11:30 CAS# C-007 Prep Batch 571222 Parameter Oil and Grease Prep Method EPA 1664A Dilution 1 Analysis Date 10/29/2015 16:18 Result 71.5 By WRW LOQ 2.0 Analytical Batch 571305 Units mg/L HACH 8000 HACH 8000 Prep Date NA CAS# C-004 Prep Batch NA Parameter COD Prep Method NA Dilution 2 Analysis Date 10/29/2015 11:28 Result 192 By DJH LOQ 10.0 Analytical Batch 571250 Units mg/L SM 2540 D-2011 SM 2540 D-2011 Prep Date NA Prep Batch NA Prep Method NA CAS# C-009 Parameter Total Suspended Solids Dilution 1 Analysis Date 10/28/2015 13:39 Result 45 By WRW LOQ 5 Analytical Batch 571208 Units mg/L GCAL Report#: 215102816 Page 13 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results SEPARATOR OUTFALL 009 SM 5210 B-2011 SM 5210 B-2011 Prep Date 10/28/2015 17:00 Prep Batch 571198 CAS# C-002 Parameter BOD Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281601 Water Prep Method BOD PREP Dilution 1 Analysis Date 10/28/2015 17:00 Result >64 By SLE LOQ 1 Analytical Batch 571527 Units mg/L UNOX EFFLUENT OUTFALL 001 UNOX EFFLUENT OUTFALL 001 EPA 624 EPA 624 Collect Date Receive Date Prep Date NA Prep Batch NA Prep Method NA CAS# 71-55-6 79-00-5 75-34-3 75-35-4 95-50-1 107-06-2 78-87-5 541-73-1 542-75-6 106-46-7 107-13-1 71-43-2 56-23-5 108-90-7 75-00-3 67-66-3 74-87-3 100-41-4 75-09-2 127-18-4 108-88-3 156-60-5 79-01-6 75-01-4 Parameter 1,1,1-Trichloroethane 1,1,2-Trichloroethane 1,1-Dichloroethane 1,1-Dichloroethene 1,2-Dichlorobenzene 1,2-Dichloroethane 1,2-Dichloropropane 1,3-Dichlorobenzene 1,3-Dichloropropylene 1,4-Dichlorobenzene Acrylonitrile Benzene Carbon tetrachloride Chlorobenzene Chloroethane Chloroform Chloromethane Ethylbenzene Methylene chloride Tetrachloroethene Toluene trans-1,2-Dichloroethene Trichloroethene Vinyl chloride 10/25/2015 19:50 10/28/2015 11:50 Dilution 1 Analysis Date 10/29/2015 05:40 Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND GCAL ID Matrix 21510281602 Water By LBH LOQ 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 10.0 5.00 20.0 5.00 2.00 5.00 5.00 5.00 5.00 5.00 10.0 5.00 5.00 5.00 5.00 5.00 Analytical Batch 571221 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L CAS# 460-00-4 1868-53-7 2037-26-5 17060-07-0 Surrogate 4-Bromofluorobenzene Dibromofluoromethane Toluene d8 1,2-Dichloroethane-d4 Conc. Spiked 30 30 30 30 Conc. Rec 29.8 28.1 31.4 29.2 Units ug/L ug/L ug/L ug/L % Recovery 99 94 105 97 Rec Limits 75 - 120 73 - 125 78 - 127 70 - 123 GCAL Report#: 215102816 Page 14 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results UNOX EFFLUENT OUTFALL 001 EPA 625 EPA 625 Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281602 Water Prep Date 10/29/2015 07:00 Prep Batch 571212 Prep Method EPA 625 Dilution 2 Analysis Date 11/04/2015 16:21 By Analytical Batch CLS 571743 CAS# 120-82-1 120-83-2 105-67-9 51-28-5 121-14-2 606-20-2 95-57-8 88-75-5 534-52-1 100-02-7 83-32-9 208-96-8 120-12-7 56-55-3 50-32-8 205-99-2 207-08-9 117-81-7 218-01-9 84-66-2 131-11-3 84-74-2 206-44-0 86-73-7 118-74-1 87-68-3 67-72-1 91-20-3 98-95-3 85-01-8 108-95-2 129-00-0 Parameter 1,2,4-Trichlorobenzene 2,4-Dichlorophenol 2,4-Dimethylphenol 2,4-Dinitrophenol 2,4-Dinitrotoluene 2,6-Dinitrotoluene 2-Chlorophenol 2-Nitrophenol 4,6-Dinitro-2-methylphenol 4-Nitrophenol Acenaphthene Acenaphthylene Anthracene Benzo(a)anthracene Benzo(a)pyrene Benzo(b)fluoranthene Benzo(k)fluoranthene Bis(2-Ethylhexyl)phthalate Chrysene Diethyl phthalate Dimethyl phthalate Di-n-butyl phthalate Fluoranthene Fluorene Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Naphthalene Nitrobenzene Phenanthrene Phenol Pyrene Result ND ND 22.2 ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND LOQ 10 10 10 10 10 10 10 10 10 10 10 10 10 5 5 10 5 10 5 10 10 10 10 10 5 10 10 10 10 10 10 10 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L CAS# 4165-60-0 321-60-8 1718-51-0 4165-62-2 367-12-4 118-79-6 Surrogate Nitrobenzene-d5 2-Fluorobiphenyl Terphenyl-d14 Phenol-d5 2-Fluorophenol 2,4,6-Tribromophenol Conc. Spiked 50 50 50 100 100 100 Conc. Rec 28.2 28.8 37.3 27.2 33.7 49.8 Units ug/L ug/L ug/L ug/L ug/L ug/L % Recovery 56 58 75 27 34 50 Rec Limits 43 - 120 16 - 128 43 - 138 10 - 120 10 - 120 19 - 133 GCAL Report#: 215102816 Page 15 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results UNOX EFFLUENT OUTFALL 001 EPA 200.8 EPA 200.8 Prep Date 11/02/2015 09:30 Prep Batch 571482 CAS# 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-24-6 7440-28-0 7440-31-5 7440-32-6 7440-66-6 7440-67-7 Parameter Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Strontium Thallium Tin Titanium Zinc Zirconium Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281602 Water Prep Method EPA 200.8 Dilution 1 Analysis Date 11/02/2015 13:55 Result ND ND 23.9 ND ND 5530 1.91 9.01 8.19 426 9.96 637 20.5 ND 8.22 298 ND ND 43.0 ND ND 6.69 274 ND By LWZ LOQ 2.00 1.00 1.00 0.50 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1.00 0.50 1.00 0.50 1.00 1.00 20.0 1.00 Analytical Batch 571497 Units ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L ug/L EPA 200.8 Prep Date 11/02/2015 09:30 CAS# 7429-90-5 7440-23-5 7440-62-2 Prep Batch 571482 Parameter Aluminum Sodium Vanadium Prep Method EPA 200.8 Dilution 10 Analysis Date 11/02/2015 13:45 Result 2230 29700 256 By LWZ LOQ 25.0 1000 10.0 Analytical Batch 571497 Units ug/L ug/L ug/L GCAL Report#: 215102816 Page 16 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Sample Results UNOX EFFLUENT OUTFALL 001 EPA 245.2 EPA 245.2 Prep Date 11/02/2015 09:45 Prep Batch 571481 CAS# 7439-97-6 Parameter Mercury Collect Date Receive Date 10/25/2015 19:50 10/28/2015 11:50 GCAL ID Matrix 21510281602 Water Prep Method EPA 245.2 Dilution 1 Analysis Date 11/02/2015 14:16 Result ND By LWZ LOQ 0.00020 Analytical Batch 571521 Units mg/L EPA 1664A EPA 1664A Prep Date 10/29/2015 11:30 CAS# C-007 Prep Batch 571222 Parameter Oil and Grease Prep Method EPA 1664A Dilution 1 Analysis Date 10/29/2015 16:18 Result 2.7 By WRW LOQ 2.0 Analytical Batch 571305 Units mg/L HACH 8000 HACH 8000 Prep Date NA CAS# C-004 Prep Batch NA Parameter COD Prep Method NA Dilution 2 Analysis Date 10/29/2015 11:28 Result 101 By DJH LOQ 10.0 Analytical Batch 571250 Units mg/L SM 2540 D-2011 SM 2540 D-2011 Prep Date NA Prep Batch NA Prep Method NA CAS# C-009 Parameter Total Suspended Solids Dilution 1 Analysis Date 10/29/2015 10:03 Result 117 By WRW LOQ 5 Analytical Batch 571269 Units mg/L SM 5210 B-2011 SM 5210 B-2011 Prep Date 10/28/2015 17:00 Prep Batch 571198 CAS# C-002 Parameter BOD Prep Method BOD PREP Dilution 1 Analysis Date 10/28/2015 17:00 Result 111 By SLE LOQ 1 Analytical Batch 571527 Units mg/L GCAL Report#: 215102816 Page 17 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 QC Summary GC/MS Volatiles QC Summary GC/MS Volatiles Analytical Batch 571221 EPA 624 1,1,1-Trichloroethane 1,1,2-Trichloroethane 1,1-Dichloroethane 1,1-Dichloroethene 1,2-Dichlorobenzene 1,2-Dichloroethane 1,2-Dichloropropane 1,3-Dichlorobenzene 1,3-Dichloropropylene 1,4-Dichlorobenzene Acrylonitrile Benzene Carbon tetrachloride Chlorobenzene Chloroethane Chloroform Chloromethane Ethylbenzene Methylene chloride Tetrachloroethene Toluene trans-1,2-Dichloroethene Trichloroethene Vinyl chloride Surrogate 1,2-Dichloroethane-d4 4-Bromofluorobenzene Dibromofluoromethane Toluene d8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix 71-55-6 79-00-5 75-34-3 75-35-4 95-50-1 107-06-2 78-87-5 541-73-1 542-75-6 106-46-7 107-13-1 71-43-2 56-23-5 108-90-7 75-00-3 67-66-3 74-87-3 100-41-4 75-09-2 127-18-4 108-88-3 156-60-5 79-01-6 75-01-4 MB571221 1503832 MB NA 10/28/2015 22:13 Water Units Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 17060-07-0 31 460-00-4 26 1868-53-7 32.4 2037-26-5 31.1 ug/L LOQ 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 5.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 LCS571221 1503833 LCS NA 10/28/2015 21:32 Water Spike Result %R Added 20.0 18.7 94 20.0 17.6 88 20.0 18.5 93 20.0 18.8 94 20.0 19.9 100 20.0 17.1 86 20.0 18.9 95 20.0 19.1 96 40.0 35.7 89 20.0 19.0 95 100 105 105 20.0 18.6 93 20.0 19.2 96 20.0 18.3 92 20.0 21.9 110 20.0 17.9 90 20.0 19.2 96 20.0 19.3 97 20.0 17.0 85 20.0 18.6 93 20.0 17.7 89 20.0 18.0 90 20.0 19.0 95 20.0 19.5 98 Control Limits%R 75 - 125 71 - 129 73 - 128 51 - 150 63 - 137 68 - 132 34 - 166 73 - 127 74 - 128 63 - 137 57 - 145 64 - 136 73 - 127 66 - 134 38 - 162 68 - 133 1 - 204 59 - 141 61 - 140 74 - 127 75 - 126 70 - 131 67 - 134 4 - 196 103 30 31.4 105 70 - 123 87 30 29.9 100 75 - 120 108 30 30 100 73 - 125 104 30 30 100 78 - 127 Analytical Batch 571221 EPA 624 Benzene Ethylbenzene Toluene Trichloroethene Surrogate 1,2-Dichloroethane-d4 4-Bromofluorobenzene Dibromofluoromethane Toluene d8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix 71-43-2 100-41-4 108-88-3 79-01-6 OUTFALL 001 21510212707 SAMPLE NA 10/29/2015 00:14 Water Units Result 1.55 0.00 1.51 1.73 17060-07-0 32 460-00-4 27.6 1868-53-7 32.6 2037-26-5 30.5 ug/L LOQ 1.00 1.00 1.00 1.00 1501242MS 1503916 MS NA 10/29/2015 00:34 Water Spike Result %R Added 20.0 20.5 95 20.0 21.0 105 20.0 19.3 89 20.0 21.4 98 Control Limits%R 37 - 151 37 - 162 47 - 150 71 - 157 107 30 31.5 105 70 - 123 92 30 28.5 95 75 - 120 109 30 30.9 103 73 - 125 102 30 28.8 96 78 - 127 GCAL Report#: 215102816 Page 18 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 GC/MS Semi-Volatiles QC Summary GC/MS Semi-Volatiles Analytical Batch 571258 Prep Batch 571212 Prep Method EPA 3510C EPA 625 1,2,4-Trichlorobenzene 2,4-Dichlorophenol 2,4-Dimethylphenol 2,4-Dinitrophenol 2,4-Dinitrotoluene 2,6-Dinitrotoluene 2-Chlorophenol 2-Nitrophenol 4,6-Dinitro-2-methylphenol 4-Nitrophenol Acenaphthene Acenaphthylene Anthracene Benzo(a)anthracene Benzo(a)pyrene Benzo(b)fluoranthene Benzo(k)fluoranthene Bis(2-Ethylhexyl)phthalate Chrysene Diethyl phthalate Dimethyl phthalate Di-n-butyl phthalate Fluoranthene Fluorene Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Naphthalene Nitrobenzene Phenanthrene Phenol Pyrene Surrogate 2,4,6-Tribromophenol 2-Fluorobiphenyl 2-Fluorophenol Nitrobenzene-d5 Phenol-d5 Terphenyl-d14 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix 120-82-1 120-83-2 105-67-9 51-28-5 121-14-2 606-20-2 95-57-8 88-75-5 534-52-1 100-02-7 83-32-9 208-96-8 120-12-7 56-55-3 50-32-8 205-99-2 207-08-9 117-81-7 218-01-9 84-66-2 131-11-3 84-74-2 206-44-0 86-73-7 118-74-1 87-68-3 67-72-1 91-20-3 98-95-3 85-01-8 108-95-2 129-00-0 MB571212 1503681 MB 10/29/2015 07:00 10/29/2015 13:26 Water Units Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND 118-79-6 73.2 321-60-8 40.7 367-12-4 40.1 4165-60-0 38.9 4165-62-2 25.7 1718-51-0 50.2 ug/L LOQ 5 5 5 5 5 5 5 5 5 5 5 5 5 3 3 5 3 5 3 5 5 5 5 5 3 5 5 5 5 5 5 5 LCS571212 1503682 LCS 10/29/2015 07:00 10/29/2015 13:43 Water Spike Result %R Added 50.0 41.9 84 50.0 48.0 96 50.0 45.4 91 50.0 42.7 85 50.0 50.5 101 50.0 51.7 103 50.0 43.4 87 50.0 51.5 103 50.0 48.1 96 50.0 20.5 41 50.0 48.8 98 50.0 51.0 102 50.0 54.6 109 50.0 55.4 111 50.0 61.4 123 50.0 63.1 126 50.0 61.4 123 50.0 65.9 132 50.0 53.0 106 50.0 52.8 106 50.0 50.4 101 50.0 59.2 118 50.0 52.5 105 50.0 49.7 99 50.0 52.4 105 50.0 39.9 80 50.0 40.1 80 50.0 43.1 86 50.0 49.4 99 50.0 51.2 102 50.0 19.6 39 50.0 57.3 115 Control Limits%R 44 - 142 39 - 135 32 - 119 1 - 191 39 - 139 50 - 158 23 - 134 27 - 182 1 - 181 1 - 132 47 - 145 33 - 145 27 - 133 33 - 143 17 - 163 24 - 159 11 - 162 8 - 158 17 - 168 1 - 114 1 - 112 1 - 118 26 - 137 59 - 121 1 - 152 24 - 116 40 - 113 21 - 133 35 - 180 54 - 120 5 - 112 52 - 115 LCSD571212 1503683 LCSD 10/29/2015 07:00 10/29/2015 13:59 Water Spike Result %R Added 50.0 40.2 80 50.0 46.9 94 50.0 45.8 92 50.0 44.6 89 50.0 49.1 98 50.0 51.9 104 50.0 45.3 91 50.0 52.0 104 50.0 49.4 99 50.0 22.1 44 50.0 47.7 95 50.0 49.7 99 50.0 54.2 108 50.0 55.6 111 50.0 60.9 122 50.0 62.2 124 50.0 61.9 124 50.0 64.2 128 50.0 53.4 107 50.0 50.1 100 50.0 49.5 99 50.0 56.6 113 50.0 51.8 104 50.0 48.3 97 50.0 52.6 105 50.0 38.6 77 50.0 39.4 79 50.0 42.2 84 50.0 49.0 98 50.0 50.5 101 50.0 21.8 44 50.0 56.7 113 RPD 4 2 1 4 3 0 4 1 3 8 2 3 1 0 1 1 1 3 1 5 2 4 1 3 0 3 2 2 1 1 11 1 RPD Limit 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 40 73 100 93.3 93 19 - 133 81 50 47.8 96 16 - 128 40 100 52.9 53 10 - 120 78 50 46.6 93 43 - 120 26 100 38.6 39 10 - 120 100 50 59.9 120 43 - 138 100 92.7 93 1 NA 50 48.7 97 2 NA 100 56.5 57 7 NA 50 46.6 93 0 NA 100 42 42 8 NA 50 60.4 121 1 NA Analytical Batch 571258 Prep Batch 571212 Prep Method EPA 3510C EPA 625 2,4-Dinitrotoluene Hexachlorobenzene Hexachlorobutadiene Hexachloroethane Nitrobenzene Surrogate 2,4,6-Tribromophenol 2-Fluorobiphenyl 2-Fluorophenol Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix 121-14-2 118-74-1 87-68-3 67-72-1 98-95-3 MUD DUMPSTER 21510274101 SAMPLE 10/29/2015 07:00 10/29/2015 17:56 Solid Units Result 0.00 0.00 0.00 0.00 0.00 118-79-6 0 321-60-8 0 367-12-4 0 ug/L LOQ 250 130 250 250 250 1503231MS 1503684 MS 10/29/2015 07:00 10/29/2015 18:29 Solid Spike Result %R Added 250 205 82 250 276 110 250 225 90 250 221 88 250 252 101 Control Limits%R - 1503231MSD 1503685 MSD 10/29/2015 07:00 10/29/2015 18:46 Solid Spike Result %R Added 250 202 81 250 274 110 250 240 96 250 237 95 250 260 104 RPD 1 1 6 7 3 RPD Limit 0* 500 380 76 - 0* 250 234 94 - 0* 500 287 57 - 500 381 76 0 NA 250 245 98 5 NA 500 294 59 2 NA GCAL Report#: 215102816 Page 19 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 GC/MS Semi-Volatiles QC Summary Analytical Batch 571258 Prep Batch 571212 Prep Method EPA 3510C EPA 625 Nitrobenzene-d5 Phenol-d5 Terphenyl-d14 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix 4165-60-0 4165-62-2 1718-51-0 MUD DUMPSTER 21510274101 SAMPLE 10/29/2015 07:00 10/29/2015 17:56 Solid Units Result 0 0 0 ug/L LOQ 0* 0* 0* 1503231MS 1503684 MS 10/29/2015 07:00 10/29/2015 18:29 Solid Spike Result %R Added 250 222 89 500 205 41 250 282 113 Control Limits%R - 1503231MSD 1503685 MSD 10/29/2015 07:00 10/29/2015 18:46 Solid Spike Result %R Added 250 239 96 500 204 41 250 284 114 RPD 7 1 1 RPD Limit NA NA NA GCAL Report#: 215102816 Page 20 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Inorganics QC Summary Inorganics Analytical Batch 571521 Prep Batch 571481 Prep Method EPA 245.2 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 245.2 Mercury 7439-97-6 MB571481 1504854 MB 11/02/2015 09:45 11/02/2015 14:09 Water Units Result ND mg/L LOQ 0.00020 LCS571481 1504855 LCS 11/02/2015 09:45 11/02/2015 14:11 Water Spike Result %R Added 0.0050 0.0055 109 Control Limits%R 80 - 120 Analytical Batch 571521 Prep Batch 571481 Prep Method EPA 245.2 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 245.2 Mercury 7439-97-6 OUTFALL 001 21510285201 SAMPLE 11/02/2015 09:45 11/02/2015 14:18 Water Units Result 0.0 mg/L LOQ 0.00020 1503676MS 1504444 MS 11/02/2015 09:45 11/02/2015 14:20 Water Spike Result %R Added 0.0050 0.0056 112 Control Limits%R 80 - 120 1503676MSD 1504445 MSD 11/02/2015 09:45 11/02/2015 14:22 Water Spike Result %R RPD RPD Added Limit 0.0050 0.0056 112 0 20 Analytical Batch 571497 Prep Batch 571171 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Sodium Strontium Thallium Tin Titanium Vanadium Zinc Zirconium 7429-90-5 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-23-5 7440-24-6 7440-28-0 7440-31-5 7440-32-6 7440-62-2 7440-66-6 7440-67-7 MB571171 1503421 MB 10/28/2015 15:15 11/02/2015 10:26 Water Units Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ug/L LOQ 2.50 2.00 1.00 1.00 0.50 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1.00 0.50 100 1.00 0.50 1.00 1.00 1.00 20.0 1.00 LCS571171 1503422 LCS 10/28/2015 15:15 11/02/2015 09:56 Water Spike Result %R Added 1000 1010 101 100 103 103 50.0 49.8 100 50.0 50.2 100 50.0 50.0 100 50.0 51.1 102 25000 25700 103 50.0 50.5 101 50.0 51.0 102 50.0 52.4 105 5000 5060 101 50.0 51.0 102 5000 5220 104 50.0 49.5 99 50.0 51.0 102 100 103 103 5000 5140 103 10.0 9.60 96 50.0 50.2 100 5000 5180 104 50.0 51.2 102 50.0 52.0 104 50.0 50.2 100 50.0 50.1 100 50.0 50.2 100 1000 1000 100 10.0 10.5 105 Control Limits%R 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 GCAL Report#: 215102816 Page 21 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Inorganics QC Summary Analytical Batch 571497 Prep Batch 571171 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Sodium Strontium Thallium Tin Titanium Vanadium Zinc Zirconium 7429-90-5 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-23-5 7440-24-6 7440-28-0 7440-31-5 7440-32-6 7440-62-2 7440-66-6 7440-67-7 WEEKLY 001A (COMP) 21510282302 SAMPLE 10/28/2015 15:15 11/02/2015 14:58 Water Units Result 107 0.53 1.54 32.4 0.0 0.0 10600 6.97 0.0 4.20 154 0.67 1220 49.4 13.4 0.61 4970 0.0 0.0 140000 154 0.0 0.0 5.52 1.58 33.1 0.38 ug/L LOQ 2.50 2.00 1.00 1.00 0.50 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1.00 0.50 100 1.00 0.50 1.00 1.00 1.00 20.0 1.00 1503585MS 1503704 MS 10/28/2015 15:15 11/02/2015 15:01 Water Spike Added Result %R 1000 1220 111 100 110 109 50.0 53.8 105 50.0 84.9 105 50.0 50.9 102 50.0 52.4 105 25000 37200 107 50.0 59.1 104 50.0 52.8 106 50.0 57.3 106 5000 5390 105 50.0 54.3 107 5000 6520 106 50.0 98.9 99 50.0 67.3 108 100 104 104 5000 10100 103 10.0 10.2 102 50.0 51.1 102 5000 143000 69* 50.0 204 99 50.0 53.8 108 50.0 53.1 106 50.0 58.6 106 50.0 54.3 106 1000 1060 103 10.0 9.62 92 Control Limits%R 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 1503585MSD 1503705 MSD 10/28/2015 15:15 11/02/2015 15:05 Water Spike Added Result %R RPD RPD Limit 1000 1270 116 4 20 100 112 112 2 20 50.0 55.7 108 3 20 50.0 86.9 109 2 20 50.0 52.5 105 3 20 50.0 54.2 108 3 20 25000 38400 111 3 20 50.0 60.8 108 3 20 50.0 54.2 108 3 20 50.0 59.7 111 4 20 5000 5610 109 4 20 50.0 55.7 110 3 20 5000 6800 112 4 20 50.0 102 105 3 20 50.0 69.1 111 3 20 100 108 107 4 20 5000 10300 107 2 20 10.0 10.6 106 4 20 50.0 52.6 105 3 20 5000 145000 114 1 20 50.0 207 105 1 20 50.0 56.0 112 4 20 50.0 54.8 110 3 20 50.0 60.7 110 4 20 50.0 56.1 109 3 20 1000 1090 106 3 20 10.0 9.96 96 3 20 Analytical Batch 571497 Prep Batch 571482 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Aluminum Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Sodium Strontium 7429-90-5 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-23-5 7440-24-6 MB571482 1504856 MB 11/02/2015 09:30 11/02/2015 13:18 Water Units Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ug/L LOQ 2.50 2.00 1.00 1.00 0.50 1.00 500 1.00 1.00 1.00 100 1.00 100 5.00 1.00 2.00 100 1.00 0.50 100 1.00 LCS571482 1504857 LCS 11/02/2015 09:30 11/02/2015 13:21 Water Spike Result %R Added 1000 1060 106 100 109 109 50.0 51.8 104 50.0 52.7 105 50.0 53.5 107 50.0 53.4 107 25000 26700 107 50.0 52.1 104 50.0 53.1 106 50.0 54.4 109 5000 5280 106 50.0 53.7 107 5000 5480 110 50.0 51.7 103 50.0 53.1 106 100 106 106 5000 5390 108 10.0 10.6 106 50.0 53.7 107 5000 5490 110 50.0 53.6 107 Control Limits%R 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 GCAL Report#: 215102816 Page 22 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 Inorganics QC Summary Analytical Batch 571497 Prep Batch 571482 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Thallium Tin Titanium Vanadium Zinc Zirconium 7440-28-0 7440-31-5 7440-32-6 7440-62-2 7440-66-6 7440-67-7 MB571482 1504856 MB 11/02/2015 09:30 11/02/2015 13:18 Water Units Result ND ND ND ND ND ND ug/L LOQ 0.50 1.00 1.00 1.00 20.0 1.00 LCS571482 1504857 LCS 11/02/2015 09:30 11/02/2015 13:21 Water Spike Result %R Added 50.0 54.3 109 50.0 52.0 104 50.0 51.4 103 50.0 51.6 103 1000 1050 105 10.0 10.9 109 Control Limits%R 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 85 - 115 Analytical Batch 571497 Prep Batch 571482 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Antimony Arsenic Barium Beryllium Cadmium Calcium Chromium Cobalt Copper Iron Lead Magnesium Manganese Molybdenum Nickel Potassium Selenium Silver Strontium Thallium Tin Titanium Zinc Zirconium 7440-36-0 7440-38-2 7440-39-3 7440-41-7 7440-43-9 7440-70-2 7440-47-3 7440-48-4 7440-50-8 7439-89-6 7439-92-1 7439-95-4 7439-96-5 7439-98-7 7440-02-0 7440-09-7 7782-49-2 7440-22-4 7440-24-6 7440-28-0 7440-31-5 7440-32-6 7440-66-6 7440-67-7 UNOX EFFLUENT OUTFALL 0.. 21510281602 SAMPLE 11/02/2015 09:30 11/02/2015 13:55 Water Units ug/L Result LOQ 0.50 2.00 0.58 1.00 23.9 1.00 0.0 0.50 0.0 1.00 5530 500 1.91 1.00 9.01 1.00 8.19 1.00 426 100 9.96 1.00 637 100 20.5 5.00 0.84 1.00 8.22 2.00 298 100 0.0 1.00 0.0 0.50 43.0 1.00 0.0 0.50 0.0 1.00 6.69 1.00 274 20.0 0.0 1.00 1503569MS 1504858 MS 11/02/2015 09:30 11/02/2015 13:58 Water Spike Result %R Added 100 97.0 96 50.0 47.5 94 50.0 89.5 131* 50.0 47.6 95 50.0 48.2 96 25000 41100 142* 50.0 51.2 98 50.0 63.8 110 50.0 68.6 121 5000 5680 105 50.0 66.0 112 5000 6180 111 50.0 98.7 156* 50.0 48.7 96 100 109 101 5000 5620 106 10.0 9.34 93 50.0 46.9 94 50.0 121 157* 50.0 49.5 99 50.0 48.1 96 50.0 63.9 114 1000 1460 119 10.0 7.64 76 Control Limits%R 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 70 - 130 1503569MSD 1504859 MSD 11/02/2015 09:30 11/02/2015 14:02 Water Spike Result %R Added 100 93.9 93 50.0 47.3 93 50.0 90.5 133* 50.0 46.7 93 50.0 47.9 96 25000 39900 137* 50.0 51.5 99 50.0 65.4 113 50.0 70.1 124 5000 6040 112 50.0 66.3 113 5000 6150 110 50.0 88.9 137* 50.0 47.9 94 100 110 102 5000 5490 104 10.0 9.10 91 50.0 46.4 93 50.0 121 156* 50.0 48.2 96 50.0 45.8 92 50.0 69.8 126 1000 1450 117 10.0 6.83 68* RPD 3 0 1 2 1 3 1 2 2 6 1 1 10 2 1 2 3 1 0 3 5 9 1 11 RPD Limit 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 20 Analytical Batch 571497 Prep Batch 571482 Prep Method EPA 200.8 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix EPA 200.8 Aluminum Sodium Vanadium 7429-90-5 7440-23-5 7440-62-2 UNOX EFFLUENT OUTFALL 0.. 21510281602 SAMPLE 11/02/2015 09:30 11/02/2015 13:45 Water Units ug/L Result LOQ 2230 25.0 29700 1000 256 10.0 1503569MS 1504858 MS 11/02/2015 09:30 11/02/2015 13:48 Water Spike Result %R Added 1000 5020 279* 5000 53400 473* 50.0 469 425* Control Limits%R 70 - 130 70 - 130 70 - 130 1503569MSD 1504859 MSD 11/02/2015 09:30 11/02/2015 13:51 Water Spike Result %R Added 1000 5550 332* 5000 53900 484* 50.0 475 439* RPD 10 1 1 RPD Limit 20 20 20 GCAL Report#: 215102816 Page 23 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 General Chemistry QC Summary General Chemistry Analytical Batch 571527 Prep Batch 571198 Prep Method BOD PREP Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 5210 B-2011 BOD C-002 MB571198 1503565 MB 10/28/2015 17:00 10/28/2015 17:00 Water Units Result ND mg/L LOQ 1 LCS571198 1503566 LCS 10/28/2015 17:00 10/28/2015 17:00 Water Spike Result %R Added 198 180 91 Control Limits%R 84.5 - 115.5 Analytical Batch 571527 Prep Batch 571198 Prep Method BOD PREP Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 5210 B-2011 BOD C-002 001 OUTFALL (COMP) 21510280201 SAMPLE 10/28/2015 17:00 10/28/2015 17:00 Water Units Result 14 mg/L LOQ 1 1503408DUP 1503567 DUP 10/28/2015 17:00 10/28/2015 17:00 Water Result RPD 13 7 RPD Limit 30 Analytical Batch 571250 HACH 8000 COD Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix C-004 MB571250 1503923 MB NA 10/29/2015 11:23 Water Units Result ND mg/L LOQ 5.0 LCS571250 1503924 LCS NA 10/29/2015 11:17 Water Spike Result %R Added 75.0 80.2 107 Control Limits%R 90 - 110 Analytical Batch 571250 HACH 8000 COD Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix C-004 102 21510281501 SAMPLE NA 10/29/2015 11:25 Water Units Result 26.0 mg/L LOQ 10.0 1503550DUP 1503925 DUP NA 10/29/2015 11:26 Water Result RPD 23.4 11 RPD Limit 20 1503550MS 1503926 MS NA 10/29/2015 11:26 Water Spike Result %R Added 150 176 100 Control Limits%R 90 - 110 Analytical Batch 571305 Prep Batch 571222 Prep Method EPA 1664A EPA 1664A Oil and Grease Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix C-007 MB571222 1503835 MB 10/29/2015 11:30 10/29/2015 16:18 Water Units Result ND mg/L LOQ 2.0 LCS571222 1503836 LCS 10/29/2015 11:30 10/29/2015 16:18 Water Spike Result %R Added 40.0 39.9 100 Control Limits%R 78 - 114 LCSD571222 1503837 LCSD 10/29/2015 11:30 10/29/2015 16:18 Water Spike Result %R Added 40.0 41.1 103 RPD 3 RPD Limit 18 Analytical Batch 571305 Prep Batch 571222 Prep Method EPA 1664A EPA 1664A Oil and Grease Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix C-007 OUTFALL 005 21510284901 SAMPLE 10/29/2015 11:30 10/29/2015 16:18 Water Units Result 0.9 mg/L LOQ 2.0 OUTFALL 005 MS 21510284903 MS 10/29/2015 11:30 10/29/2015 16:18 Water Spike Result %R Added 40.0 40.9 100 Control Limits%R 78 - 114 OUTFALL 005 MSD 21510284904 MSD 10/29/2015 11:30 10/29/2015 16:18 Water Spike Result %R Added 40.0 34.7 84 RPD 16 RPD Limit 18 GCAL Report#: 215102816 Page 24 of 27 Report#: Project ID: 215102816 BR Chemical Plant Report Date: 11/11/2015 General Chemistry QC Summary Analytical Batch 571208 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 2540 D-2011 Total Suspended Solids C-009 MB571208 1503626 MB NA 10/28/2015 13:39 Water Units Result ND mg/L LOQ 5 LCS571208 1503627 LCS NA 10/28/2015 13:39 Water Spike Result %R Added 50 45 90 Control Limits%R 80 - 120 Analytical Batch 571208 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 2540 D-2011 Total Suspended Solids C-009 OUTFALL 202-ADMIN 21510275801 SAMPLE NA 10/28/2015 13:39 Water Units Result 4 mg/L LOQ 5 1503312DUP 1503628 DUP NA 10/28/2015 13:39 Water Result RPD 4 0 RPD Limit 5.4 Analytical Batch 571208 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 2540 D-2011 Total Suspended Solids C-009 OUTFALL 201 21510282502 SAMPLE NA 10/28/2015 13:39 Water Units Result 1 mg/L LOQ 5 1503588DUP 1503629 DUP NA 10/28/2015 13:39 Water Result RPD 1 0 RPD Limit 5.4 Analytical Batch 571269 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 2540 D-2011 Total Suspended Solids C-009 MB571269 1503999 MB NA 10/29/2015 10:03 Water Units Result ND mg/L LOQ 5 LCS571269 1504000 LCS NA 10/29/2015 10:03 Water Spike Result %R Added 50 51 102 Control Limits%R 80 - 120 Analytical Batch 571269 Client ID GCAL ID Sample Type Prep Date Analysis Date Matrix SM 2540 D-2011 Total Suspended Solids C-009 OUTFALL 001 21510276501 SAMPLE NA 10/29/2015 10:03 Water Units Result 10 mg/L LOQ 5 1503331DUP 1504001 DUP NA 10/29/2015 10:03 Water Result RPD 10 0 RPD Limit 5.4 GCAL Report#: 215102816 Page 25 of 27 GCAL Report#: 215102816 Page 26 of 27 GCAL Report#: 215102816 Page 27 of 27 ExxonMobil Baton Rouge Chemical Plant October 24, 2017 Appendix 9 - Multiple Chain of Custody Reports 13