ED Sn; e" 5% .0 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY "Quinn; 3 0 4' 'it Pact' November 20, 2012 Enbridge Energy, Limited Partnership c/o Mr. Rich Adams Vice President, Operations Superior City Centre Second Floor 1409 Hammond Ave. Superior, Wisconsin 54880 Re: U.S. EPA Directive to Complete Submerged Oil Quantification in response to the Removal Administrative Order issued by U.S. EPA on July 27, 2010, pursuant to 311(c) of the Clean Water Act (Docket No. CWA 1321-5-10-001) and Supplement to Order for Compliance issued by U.S. EPA on September 23, 2010 Dear Mr. Adams: The United States Environmental Protection Agency directs Enbridge Energy, Limited Partnership ("Enbridge") to complete the quantification of submerged oil in the sections of the Kalamazoo River affected by the Enbridge Line 6B oil spill as directed below. U.S. EPA issues this directive pursuant to paragraph 18 of the Removal Administrative Order ("Order") issued by U.S. EPA on July 27, 2010 and paragraph 6(f) ofthe Supplement to Order for Compliance under Section 311(0) of the Clean Water Act ("Supplement") issued by U.S. EPA on September 23, 2010 (Docket No. CWA 1321-5-10-001). BACKGROUND On December 21, 201 l, U.S. EPA approved the Consolidatea' Work Plan from Fall 2011 to 2012 ("2012 Consolidated Work Plan") submitted by Enbridge pursuant to the Order and the Supplement. The 2012 Consolidated Work Plan requires Enbridge to quantify the submerged oil based on sediment cores collected in the summer of 2012. Since that time, U.S. EPA and Enbridge have been developing methodologies for quantification of the submerged oil based on the forensic chemical analysis results. In August 2012, a Pilot Test was initiated after questions arose regarding the feasibility of using visualization techniques to identify Line 6B oil in sediment cores during core logging. Enbridge carried out sediment core logging for the Pilot Test according to a methodology established in Enbridge's Submerged Oil Volume Quantification (Field Guide) (Attachment 1). Enbridge also submitted the Submerged Oil Volume Quantification (Pilot Test) (Attachment 2), which governed the methodology applied to the sample processing and chemical analysis for the Pilot Test. Based on U.S EPA's interpretation of the results of the Pilot Test, shown in Attachment 3, U.S. EPA concludes that current visualization techniques are inadequate to serve as a basis for selecting core intervals for forensic chemical analysis. CORE SAMPLING AND FORENSIC CHEMICAL ANALYSIS METHODOLOGY This directive and its attachments set forth the approved methodology which Enbridge shall implement to quantify the submerged oil in the sections of the Kalamazoo River affected by the Enbridge Line 6B oil release. U.S. EPA reserves the right to supplement or modify this methodology with future directives should additional information become available that requires such a change. in accordance with this directive, Enbridge shall immediately process and analyze the sediment cores that it collected in the summer of 2012 for the purpose of quantifying submerged oil. Enbridge shall inform U.S. EPA of the time and location of all activities described herein with adequate notice in order to allow U.S. EPA to mobilize appropriate oversight personnel. In addition to complying with this requirement, Enbridge shall comply with other specific notification requirements contained in this directive. A. Sediment Cores Subiect to this Directive This directive applies to the following sets of sediment cores which Enbridge collected in the summer of 2012: 1. Previously Logged Cores Enbridge has already logged forty--eight (48) sediment cores and has collected interval samples from those cores, but has not yet analyzed those samples. These sediment samples are currently in Enbridge custody, in cold storage at Alpha Laboratory. A copy of the annotated core logs for these cores is included as Attachment 4. 2. Intact Cores Approximately forty (40) of the sediment cores are still intact and have not yet been processed to collect interval samples or analyzed. The Intact Cores are currently under cold storage in Enbridge custody and are listed in Attachment 5. 3. Pilot Test Cores Twelve (12) cores have already undergone a sampling procedure similar to that described in this directive, and have undergone forensic chemical analysis. These cores are highlighted in Attachment 4. These cores may be subject to additional sampling and analysis as described in Section B.4 below. 13. Core Interval Sample Collection and Sample Preparation Enbridge shall use the following protocol to identify sediment core sample intervals that it must analyze pursuant to this directive and to collect and prepare those samples for analysis. Enbridge shall provide U.S. EPA with at least three (3) days notice prior to commencing core logging or sample preparation. Enbridge shall complete processing of all Previously Logged Cores and intact Cores no later than December 7, 2012. 1. Previously Logged Cores Enbridge will process the samples from the Previously Logged cores, identified in Section A.l above, according to the methodology set forth in Attachment 2, with the following modifications: 2. Intact Cores Enbridge will submit for analysis all sample intervals identified on the corresponding core log included in Attachment 4. Enbridge is not required to send the samples to Dr. Kenneth Lee or have them analyzed using epifluorescence microscopy. Enbridge shall process the intact Cores in the manner prescribed in the Core Processing section of Attachment 1, with the following modifications: Et. Enbridge shall process the primary core labeled Core #1 from each location; the primary core labeled Core #2 shall be retained and maintained in cold storage. Enbridge shall split Core #1 and perform logging of one half of Core #1 following the procedure described in Attachment 1. Enbridge shall process the unlogged half of Core by doing the following: i) Enbridge shall collect the top l--ir1ch of the core in a separate container; and ii) Enbridge shall collect all remaining stratigraphic layers into appropriately sized sample containers at a maximum of up to 6 inches of core material per container. Enbridge shall analyze a sample from the topmost 1-inch interval of the first depositional layer of sediment from each Intact Core; Enbridge shall analyze multiple sediment samples comprising the full thickness of the first depositional layer below the top--inch interval; each sediment sample shall be collected from an interval of no greater than six inches of the sediment core material. Enbridge shall collect a separate sample for any core interval (regardless of depth and/or lithology) in which visible oil is found. Enbridge shall process core samples for laboratory analysis by homogenizing discrete intervals and performing subsampling using the incremental Sampling Method (aliquot cornpositing), as described in Attachment 2. Enbridge shall retain all core sample intervals not analyzed in cold storage until otherwise directed by U.S. EPA. Enbridge shall provide copies of completed core logs to US. EPA for all Intact Cores that clearly identify all sample interval depths and sample label designations on a rolling basis within 5 days following the core logging. All com_pleted core logs shall be provided to U.S. EPA no later than "December 14, 2012. j. Enbridge is not required to send the samples to Dr. Kenneth Lee or analyze them using epifluorescence microscopy. 3. Reference Samples Upon completion of logging of the Intact Cores, Enbridge shall also collect representative samples of the lower depositional layers of an estimated 10 -- 12 cores selected from all cores identified in Section A of this directive. Enbridge will select these cores on the basis of completed core logs after approval by U.S. EPA. Enbridge will process these additional samples in the manner described in Attachment 2 and shall submit them for forensic chemical analysis in accordance with Section below. 4. Additional Samples U.S. EPA may require Enbridge to conduct additional sampling after review of the analytical results submitted by Enbridge pursuant to Sections C.l and C.2 below. For any sediment core in which the Enbridge Line 68 oil concentration within the initially lowermost sample is above the method detection limit identified in the written methodology, which U.S. EPA will provide (See Section C.3. below), Enbridge shall submit additional deeper samples from that core for forensic chemical analysis. Enbridge shall collect samples of the next lower depositional layer in such sediment core and shall process those additional samples according to the methodology provided in Attachment 2. Enbridge will select these samples after consultation with and approval by U.S. EPA. Enbridge will continue this procedure for such core until analytical results identify a layer that yields a concentration of Line 68 oil below the method detection limit. C. Laboratory Analysis (All Cores) Enbridge shall implement the forensic chemical analysis of all samples required by Sections A and of this directive as set forth in this Section. As described in Section 8.4, if additional samples are required, Enbridge shall also analyze them in accordance with this section. Enbridge shall complete the laboratory analyses described in Sections and C.2 no later than January 25, 2013. Enbridge shall submit the analytical results to U.S. EPA on a rolling basis as they come in, but no later than January 25, 2013. 1. Quality Assurance Project Plan Enbridge shall provide a copy of the QAPP it is currently using to U.S. EPA within 5 working days of receipt of this directive. U.S. EPA will advise Enbridge if any further modifications to the QAPP are required prior to the start of the chemical analyses required by this directive. Enbridge shall continue processing samples in accordance with Section above according to the schedule set forth below. 2. Total Oil Analysis In accordance with the QAPP required by Section C.1 above, Enbridge shall analyze the samples identified in Section for alkylated PNAS, biomarkers, and saturated hydrocarbons. 3. Oil Source Identification After review of the final analytical results, US. EPA will provide in writing to Enbridge a methodology to determine the concentration of Line 6B oil in the samples. Enbridge shall apply that methodology to the analytical results of each sample identified in Section and submit its results to US. EPA within ten (10) days as part of the revised Submerged Oil Quantification Report (see Section below). D. Reporting Requirements Enbridge shall revise the Submerged Oil Quantification Report dated May 4, 2012 (Attachment 6) to reflect the results obtained pursuant to this directive within ten (10) days of receipt of the Oil Source Identification methodology described in Section C.3. The revised report shall include: 1. Statistical Evaluation Enbridge shall use the approach described in the August 8, 2012 letter from Thomas Graan (Scientific Support Coordinator) to Ralph Dollhopf (Federal On--Scene Coordinator) (Attachment 7) to develop representative Line 6B oil concentrations (and associated uncertainties) for each geomorphic stratum. 2. Oil Volume Calculator Enbridge shall calculate the quantity of Line 6B submerged oil using the procedure and process described in Attachment 6 using the oil concentration methodology developed from Section C.3 above and Late Summer Reassessment (LSR) 2012 poling results. SCHEDULE U.S. EPA directs Enbridge to complete the activities described above according to the following schedule: I Enbridge shall submit the QAPP to U.S. EPA within five (5) working days of receipt of this directive. 0 Enbridge shall complete processing of the Previously Logged Cores and the Intact Cores, for forensic chemical analysis as set forth in Section no later than December 7, 2012. 0 Enbridge shall provide copies of all completed core logs to US EPA no later than December 14, 2012. I Enbridge shall complete all analyses as described in Sections C.l and C2, including all Quality Assurance/Quality Control samples and review, and receive final analytical results for quantification of submerged oil using the summer of 201 2 core samples by January 25, 2013. 0 Enbridge shall submit final analytical results described in the bullet above to U.S. EPA on a rolling basis as they become available, but no later than January 25, 2013. 0 After review of the final analytical results obtained pursuant to Sections C.1 and C.2, U.S. EPA shall provide Enbridge with a methodology for determining the concentration of Line 6B oil in the samples as set forth in Section C.3 and notify Enbridge if the additional sampling described in Section B.4 is required. 0 Within ten (10) days of receipt of the methodology described in the bullet above, Enbridge shall submit a revised Submerged Oil Quantification Report in accordance with Section D. Please contact me immediately at (734) 308-1695 if you have any questions or require clarification to ensure that the schedule requirements described herein are achieved. Sincerely, Jeffrey Lippert Acting Federal On-Scene Coordinator U.S. EPA, Region 5 Attachments cc: L. Kirby-Miles, U.S. EPA, ORC K. Peaceman, U.S. EPA, ORC C. Mikalian, U.S. EPA, ORC S. l\/IcAnaney, U.S. EPA, ORC M. DeLong, MDEQ Records Center, EPA, Reg.