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I:\WO\START3\1269\44215TechMemo.docx 1 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA. It shall not be released or disclosed in whole or in part without the express written permission of U.S. EPA. TO: Brenda Jones, Task Monitor, United States Environmental Protection Agency (U.S. EPA), Region 5, Great Lakes National Program Office (GLNPO) FROM: Alexandra Clark, Project Manager, Weston Solutions, Inc. (WESTON ® ), Superfund Technical Assessment and Response Team (START) SUBJECT: Technical Memorandum for October 2011 Otter Creek Confluence Data Duck and Otter Creeks Confluence Investigation Toledo, Lucas County, Ohio DATE: February 10, 2012 As requested by the U.S. EPA GLNPO, WESTON prepared this technical memorandum to summarize sediment investigation activities conducted in October 2011 at the confluence of Otter Creek with Maumee Bay in Toledo, Lucas County, Ohio (the Site; see Figure 1 in Attachment A). The investigation activities were conducted as supplemental work to the November 2010 and May 2011 sediment sampling investigations to further define the horizontal extent of contamination at the confluence of Otter Creek with Maumee Bay. October 2011 sediment sampling activities were conducted in accordance with WESTON’s “Quality Assurance Project Plan (QAPP), Amendment 2,” and “Field Sampling Plan (FSP), Amendment 3,” dated September 2011. GLNPO, WESTON, and the crew of the Research Vessel Mudpuppy 2 mobilized to the Site on October 17, 2011. However, sampling could not be conducted that day because of high wind conditions on the Maumee River. On October 18, 2011, sediment sampling was conducted. Figure 2 in Attachment A shows the 13 sampling locations. Table 1 in Attachment B lists the sampling location coordinates, water depths, core retrieval information, and visual and olfactory observations (sheen and odors). A photographic log from the October 2011 sampling is provided in Attachment C. A total of 13 (plus 1 duplicate) surface sediment grab samples were collected and analyzed as summarized in the table below. Surface Sediment Grab Sample Summary Sampling Device Parameter Laboratory Peterson grab sampler 34 polynuclear aromatic hydrocarbons (PAH) Contract Laboratory Program (CLP) Total organic carbon (TOC) Columbia Analytical Services Toxicity United States Army Corps of Engineers, Engineer Research and Development Center

TO: Brenda Jones, Task Monitor, United States ... · I:\WO\START3\1269\44215TechMemo.docx 3 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA

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Page 1: TO: Brenda Jones, Task Monitor, United States ... · I:\WO\START3\1269\44215TechMemo.docx 3 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA

I:\WO\START3\1269\44215TechMemo.docx 1 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA. It shall not be released or disclosed in whole or in part without the express written permission of U.S. EPA.

TO: Brenda Jones, Task Monitor, United States Environmental Protection Agency (U.S. EPA), Region 5, Great Lakes National Program Office (GLNPO)

FROM: Alexandra Clark, Project Manager, Weston Solutions, Inc. (WESTON®),

Superfund Technical Assessment and Response Team (START) SUBJECT: Technical Memorandum for October 2011 Otter Creek Confluence Data

Duck and Otter Creeks Confluence Investigation Toledo, Lucas County, Ohio

DATE: February 10, 2012

As requested by the U.S. EPA GLNPO, WESTON prepared this technical memorandum to summarize sediment investigation activities conducted in October 2011 at the confluence of Otter Creek with Maumee Bay in Toledo, Lucas County, Ohio (the Site; see Figure 1 in Attachment A). The investigation activities were conducted as supplemental work to the November 2010 and May 2011 sediment sampling investigations to further define the horizontal extent of contamination at the confluence of Otter Creek with Maumee Bay. October 2011 sediment sampling activities were conducted in accordance with WESTON’s “Quality Assurance Project Plan (QAPP), Amendment 2,” and “Field Sampling Plan (FSP), Amendment 3,” dated September 2011.

GLNPO, WESTON, and the crew of the Research Vessel Mudpuppy 2 mobilized to the Site on October 17, 2011. However, sampling could not be conducted that day because of high wind conditions on the Maumee River. On October 18, 2011, sediment sampling was conducted. Figure 2 in Attachment A shows the 13 sampling locations. Table 1 in Attachment B lists the sampling location coordinates, water depths, core retrieval information, and visual and olfactory observations (sheen and odors). A photographic log from the October 2011 sampling is provided in Attachment C. A total of 13 (plus 1 duplicate) surface sediment grab samples were collected and analyzed as summarized in the table below.

Surface Sediment Grab Sample Summary

Sampling Device Parameter Laboratory Peterson grab sampler

34 polynuclear aromatic hydrocarbons (PAH)

Contract Laboratory Program (CLP)

Total organic carbon (TOC) Columbia Analytical Services Toxicity United States Army Corps of

Engineers, Engineer Research and Development Center

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Technical Memorandum for October 2011 Otter Creek Confluence Data (Continued) Duck and Otter Creeks Confluence Investigation

I:\WO\START3\1269\44215TechMemo.docx 2 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA. It shall not be released or disclosed in whole or in part without the express written permission of U.S. EPA.

A total of 50 subsurface sediment sample cores (including duplicate and split samples) were collected and analyzed as summarized in the table below.

Subsurface Sediment Core Sample Summary

Sampling Device Parameter Laboratory Vibracore sediment corer

Semivolatile organic compounds (SVOC)

CLP

TOC Columbia Analytical Services A total of 13 pore water samples (plus 1 duplicate) were extracted from the sediment samples collected using the Peterson grab sampler at the respective laboratories and analyzed as summarized in the table below.

Pore Water Sample Summary

Sample Type Parameter Laboratory Pore water 34 PAHs University of North Dakota, Energy

and Environmental Research Center Dissolved organic carbon

(DOC) Columbia Analytical Services

Ammonia pH

Tables 2, 3 (a, b, and c), 4, and 5 in Attachment B summarize the analytical results for the sediment samples analyzed for 34 PAHs, SVOCs, and TOC as well as the pore water sample results, respectively. Table 6 summarizes the toxicity testing results for the sediment samples. The toxicity testing laboratory report is provided in Attachment D.  

A WESTON chemist performed validation of 5 percent of the subcontracted analytical data as required by GLNPO. The GLNPO data management subcontractor validated all CLP data. WESTON input all October 2011 analytical data into the existing EQuIS database and submitted the data to Great Lakes Sediment Database (GLSED) on January 10, 2012.

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Technical Memorandum for October 2011 Otter Creek Confluence Data (Continued) Duck and Otter Creeks Confluence Investigation

I:\WO\START3\1269\44215TechMemo.docx 3 1269-2B-AUGE This document was prepared by Weston Solutions, Inc., expressly for U.S. EPA. It shall not be released or disclosed in whole or in part without the express written permission of U.S. EPA.

If you have any questions regarding this submittal, please contact the undersigned at (248) 658-5015. APPROVAL AND SIGNATURE

___________________________________________________ Alexandra Clark/WESTON START Project Manager Attachments: A - Figures B - Tables C – Photographic Log D – Final Toxicity Testing Report

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ATTACHMENT A FIGURES

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DUCK CREEK CONFLUENCEPROJECT AREA

OTTER CREEKCONFLUENCEPROJECT AREA

FIGURE 1Site Location Map

Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, OhioContract No.: EP-S5-06-04TDD: S05-0008-1010-036DCN: 1269-2B-AUGE

0 2,000Feet

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Image Source: ESRI US Topo Maps

Prepared for: U.S. EPA REGION V

Prepared By:WESTONSOLUTIONS, INC

360 E MapleSuite R

Troy, Michigan 48083

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OC-48 OC-47 OC-46

OC-45

OC-44

OC-42

OC-41OC-40

OC-38

OC-36OC-35

OC-34

OC-33

OC-32

OC-31 OC-30

OC-29

OC-28

OC-27 OC-26

OC-61

OC-60OC-59OC-58

OC-57OC-56

OC-55

OC-54

OC-53

OC-52

OC-51

OC-50OC-49

FIGURE 2October 2011 Otter Creek

Confluence Sampling Locations Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, OhioContract No.: EP-S5-06-04TDD: S05-0008-1010-036DCN: 1269-2B-AUGE

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360 E MapleSuite R

Troy, Michigan 48083

Prepared For:U.S. EPA REGION V

Prepared By:WESTON SOLUTIONS

Imagery Souce: ESRI Bing Maps

Legend2011 October Sampling Locations2010 November/2011 MaySampling LocationsShipping Channel

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ATTACHMENT B TABLES

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Table 1October 2011 Sampling Data - Sampling Location Information

Duck and Otter Creeks Confluence InvestigationToledo, Lucas County, Ohio

Location ID No. Water Depth

Core Retrieval Visual and Olfactory Observations

OC-49 83°27.2876' W 41°41.9216' N 2'11" 50" Moderate petroleum odor; light sheenOC-50 83°27.2607' W 41°41.9223' N 2'6" 63" Moderate to strong petroleum odor; sheen on waterOC-51 83°27.2852' W 41°41.9637' N 3'9" 44" Petroleum odor with staining in surface sediment; slight petroleum odor in subsurface OC-52 83°27.2241' W 41°41.9438' N 2'10" 64" Strong petroleum odor and sheenOC-53 83°27.2192' W 41°41.9752' N 4'2" 32" Slight sheen; slight petroleum odorOC-54 83°27.1981' W 41°41.9555' N 3'3" 65" Sheen on confluence water surface when core retrieved; strong petroleum odorOC-55 83°27.2561' W 41°42.0033' N 4'10" 42" Slight petroleum odorOC-56 83°27.1933' W 41°41.9856' N 5'8" 112" Free oil present; strong staining; strong petroleum odorOC-57* 83°27.1537' W 41°41.9847' N 5'0" 120" Strong sheen and petroleum odorOC-58* 83°27.2200' W 41°42.0188' N 6'1" 120" No to slight petroleum odor at surface; strong petroleum odor and staining with depthOC-59* 83°27.1860' W 41°42.0218' N 5'10" 121" No to slight petroleum odor at surface; strong petroleum odor and sheen with depthOC-60* 83°27.1441' W 41°42.0122' N 6'11" 121" Strong sheen and petroleum odorOC-61* 83°27.1453' W 41°42.0486' N 8'3" 122" Slight petroleum odor; no sheen

Notes* = Did not meet core refusal; therefore, sediment thickness exceeds than 10 feet' = Foot or minute" = Inch° = DegreeID = IdentificationN = North

W = West

Sampling Location Coordinates

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This document shall not be disclosed without the express written permission of U.S. EPA 1269-2B-AUGE

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Table 2October 2011 Sampling Data - 34 PAH Results for Sediment Samples

Duck and Otter Creeks Confluence InvestigationToledo, Lucas County, Ohio

Location ID OC-49 OC-50 OC-50 OC-51 OC-52 OC-53 OC-54 OC-55 OC-56 OC-57 OC-58 OC-59 OC-60 OC-61

Field Sample ID OC-49 OC-50 OC-50-DP OC-51 OC-52 OC-53 OC-54 OC-55 OC-56 OC-57 OC-58 OC-59 OC-60 OC-61

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011

Depth Interval (in. bss)

Unit1-Methylnaphthalene µg/kg 14 6 U 6.6 5.7 U 6 U 19 42 6.3 U 1,200 J 280 J 6.8 U 5.5 J 220 J 7.6 U2-Methylnaphthalene µg/kg 36 9.6 14 6.6 10 33 70 J 11 300 J 400 J 6.8 U 12 350 J 7.6 UAcenaphthene µg/kg 5.5 U 9 15 5.7 U 10 6.8 11 6.3 U 140 J 38 6.8 U 6.3 U 280 J 7.6 UAcenaphthylene µg/kg 5.5 U 6 U 7.5 5.7 U 6 U 8 5.3 6.3 U 35 16 6.8 U 6.3 U 20 8.3Anthracene µg/kg 89 J 53 73 J 9.1 37 24 43 6.9 500 J 120 J 6.8 U 6.6 910 J 14Benzo(a)anthracene µg/kg 370 J 180 J 290 J 19 120 J 68 J 140 J 17 820 J 340 J 11 18 780 J 33Benzo(a)pyrene µg/kg 240 J 110 J 160 J 19 79 J 71 J 120 J 22 450 J 270 J 15 24 560 J 36Benzo(b)fluoranthene µg/kg 230 J 88 J 120 J 18 61 J 70 J 130 J 24 300 J 260 J 18 24 570 J 41Benzo(e)pyrene µg/kg 320 J 130 J 180 J 20 100 J 70 J 160 J 18 680 J 370 J 15 27 420 J 23Benzo(g,h,i)perylene µg/kg 170 J 61 J 88 J 13 47 50 96 J 17 200 J 200 J 12 20 270 J 22Benzo(k)fluoranthene µg/kg 31 13 20 5.7 U 12 20 20 7.1 57 J 38 6.8 U 6.6 210 J 16C1 Chrysenes µg/kg 830 J 590 J 880 J 31 J 320 J 140 J 410 J 30 J 2,400 J 1,200 J 22 J 40 J 1,000 J 13 JC1-Fluoranthenes/Pyrenes µg/kg 840 J 300 J 420 J 34 J 210 J 140 J 320 J 26 J 1,900 J 1,000 J 25 J 28 J 1,300 J 29 JC1-Fluorenes µg/kg 170 J 52 J 80 J 9.2 J 53 J 25 J 60 J 6.3 U 830 J 190 J 6.8 U 6.3 U 220 J 7.6 UC1-Naphthalenes µg/kg 33 J 6.9 J 12 J 6.6 J 8.1 J 34 J 73 J 10 J 1,000 J 450 J 6.8 U 6.4 J 370 J 7.3 JC1-Phenanthrenes/Anthracenes µg/kg 720 J 86 J 130 J 14 J 110 J 76 J 210 J 14 J 3,100 J 630 J 9.7 J 18 J 940 J 15 JC2 Chrysenes µg/kg 550 J 450 J 670 J 24 J 280 J 110 J 370 J 39 J 2,300 J 1,300 J 27 J 42 J 830 J 7.6 JC2-Fluoranthenes/Pyrenes µg/kg 490 J 330 J 460 J 23 J 210 J 110 J 310 J 29 J 1,300 J 1,400 J 24 J 31 J 830 J 14 JC2-Fluorenes µg/kg 270 J 180 J 270 J 5.3 J 140 J 40 J 120 J 6.3 U 1,400 J 270 J 6.8 U 6.3 U 310 J 7.6 UC2-Naphthalenes µg/kg 100 J 29 J 39 J 11 J 54 J 62 J 150 J 13 J 4,600 J 710 J 6.8 U 18 J 540 J 8.3 JC2-Phenanthrenes/Anthracenes µg/kg 760 J 260 J 410 J 17 J 320 J 120 J 340 J 15 J 3,100 J 1,100 J 25 J 23 J 1,000 J 7.4 JC3 Chrysenes µg/kg 150 J 150 J 370 J 11 J 73 J 85 J 150 J 22 J 1,100 J 1,200 J 6.8 U 15 J 570 J 7.6 UC3-Fluoranthenes/Pyrenes µg/kg 330 J 320 J 460 J 12 J 210 J 81 J 280 J 22 J 1,200 J 1,600 J 15 J 18 J 760 J 7.6 UC3-Fluorenes µg/kg 210 J 240 J 360 J 17 J 190 J 53 J 160 J 6.3 U 1,200 J 460 J 15 J 10 J 360 J 7.6 UC3-Naphthalenes µg/kg 520 J 120 J 160 J 14 J 250 J 88 J 220 J 8.1 J 5,300 J 800 J 6.8 U 14 J 610 J 7.6 UC3-Phenanthrenes/Anthracenes µg/kg 320 J 290 J 420 J 16 J 250 J 100 J 300 J 26 J 2,100 J 1,500 J 32 J 29 J 820 J 7.6 UC4 Chrysenes µg/kg 130 J 100 J 88 J 5.7 U 43 J 31 J 72 J 8.6 J 400 J 320 J 6.8 U 15 J 220 J 7.6 UC4-Naphthalenes µg/kg 410 J 340 J 480 J 23 J 360 J 87 J 230 J 11 J 4,100 J 770 J 9 J 14 J 570 J 7.6 UC4-Phenanthrenes/Anthracenes µg/kg 160 J 220 J 300 J 13 J 190 J 78 J 230 J 26 J 1,600 J 1,300 J 26 J 31 J 590 J 7.6 UChrysene µg/kg 810 J 300 J 410 J 27 190 J 130 J 320 J 28 900 J 630 J 20 30 860 J 36Dibenzo(a,h)anthracene µg/kg 130 J 64 J 84 J 7.7 45 29 63 J 7.4 210 J 130 J 6.8 U 11 160 J 7.6 UFluoranthene µg/kg 220 J 59 93 J 20 46 66 J 110 J 24 340 J 280 J 17 23 1,400 J 66Fluorene µg/kg 55 6 U 6.1 U 5.7 U 15 14 19 6.3 U 320 J 85 J 6.8 U 6.3 U 530 J 8.5Indeno(1,2,3-cd)pyrene µg/kg 66 J 36 48 8.5 26 31 46 13 110 J 99 J 8.8 12 220 J 21Naphthalene µg/kg 35 14 24 15 15 26 40 11 240 J 240 J 9.6 12 330 J 130 JPerylene µg/kg 25 6.2 10 7 6.4 18 18 8.6 41 46 J 6.8 U 6.8 110 J 10Phenanthrene µg/kg 360 J 22 29 12 24 54 J 130 J 14 1,200 J 500 J 11 17 1,800 J 38Pyrene µg/kg 500 J 140 J 200 J 29 100 J 90 J 190 J 24 880 J 410 J 16 22 930 J 47Total 16 PPAH µg/kg 3,300 1,100 1,700 200 840 760 1,500 220 6,700 3,700 140 230 9,800 510Total PAH µg/kg 11,000 J 5,400 J 7,900 J 510 J 4,200 J 2,300 J 5,700 J 540 J 46,000 J 20,000 J 380 J 610 J 22,000 J 650 JNotes:µg/kg = Microgram per kilogram PAH = Polycyclic aromatic hydrocarbonDP = Duplicate PPAH = Particulate polycyclic aromatic hydrocarbonID = Identification SIM = Selective Ion Monitoringin. bss = Inches below sediment surface SVOA = Semivolatile organic analysisJ = Analyte identification is acceptable; reported value is an estimate U = Compound analyzed for but not detected above reported detection limitAll samples analyzed using United States Environmental Protection Agency Method MC SVOA (SIM)

0 - 6 0 - 6

Chemical Name 1 Result

0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6 0 - 6

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This document shall not be disclosed without the express written permission of U.S. EPA

1269-2B-AUGE

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Table 3aOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-49-01 through OC-54-02Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, Ohio

Location ID OC-49 OC-49 OC-50 OC-50 OC-50 OC-51 OC-51 OC-52 OC-52 OC-52 OC-52 OC-52 OC-52 OC-53 OC-53 OC-54 OC-54Field Sample ID OC-49-01 OC-49-02 OC-50-01 OC-50-02 OC-50-03 OC-51-01 OC-51-02 OC-52-01 OC-52-01-DP OC-52-02 OC-52-02-DP OC-52-03 OC-52-03-DP OC-53-01 OC-53-02 OC-54-01 OC-54-02

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 0- 24 24- 48 0- 24 24- 48 48- 63 0- 24 24- 48 0- 24 0- 24 24- 48 24- 48 48- 64 48- 64 0- 24 24- 32 0- 24 24- 48

Unit

1,1'-Biphenyl µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 U1,2,4,5-Tetrachlorobenzene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,2'-Oxybis(1-chloropropane) µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,3,4,6-Tetrachlorophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,4,5-Trichlorophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,4,6-Trichlorophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,4-Dichlorophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,4-Dimethylphenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,4-Dinitrophenol µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 U2,4-Dinitrotoluene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2,6-Dinitrotoluene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2-Chloronaphthalene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2-Chlorophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2-Methylnaphthalene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 67 J 2,2002-Methylphenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U2-Nitroaniline µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 U2-Nitrophenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U3,3'-Dichlorobenzidine µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U3-Nitroaniline µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 U4,6-Dinitro-2-methylphenol µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 U4-Bromophenyl-phenylether µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 U4-Chloro-3-methylphenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U4-Chloroaniline µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U4-Chlorophenyl-phenylether µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 U4-Methylphenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 910 6804-Nitroaniline µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 U4-Nitrophenol µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 UAcenaphthene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UAcenaphthylene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UAcetophenone µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UAnthracene µg/kg 88 J 130 U 52 J 130 U 120 U 140 U 120 U 57 J 140 U 140 U 70 J 130 U 120 U 150 U 140 U 190 U 540Atrazine µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UBenzaldehyde µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UBenzo(a)anthracene µg/kg 480 130 U 240 130 U 120 U 140 U 120 U 320 140 160 270 130 U 120 U 150 U 140 UJ 150 J 4,000Benzo(a)pyrene µg/kg 340 130 U 180 130 U 120 U 140 U 120 U 150 J 130 J 150 300 130 U 120 U 150 U 140 UJ 140 J 3,200Benzo(b)fluoranthene µg/kg 330 130 U 140 J 130 U 120 U 140 U 120 U 110 J 94 J 150 290 130 U 120 U 150 U 140 UJ 170 J 2,200Benzo(g,h,i)perylene µg/kg 250 130 U 100 J 130 U 120 U 140 U 120 U 84 J 67 J 83 J 180 130 U 120 U 150 U 140 UJ 120 J 2,100Benzo(k)fluoranthene µg/kg 100 J 130 U 70 J 130 U 120 U 140 U 120 U 56 J 140 U 53 J 160 130 U 120 U 150 U 140 UJ 190 U 2,000Bis(2-chloroethoxy)methane µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UBis(2-chloroethyl)ether µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UBis(2-ethylhexyl)phthalate µg/kg 58 J 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 240Butylbenzylphthalate µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UCaprolactam µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UCarbazole µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UChrysene µg/kg 1,400 130 U 490 130 U 120 U 140 U 120 U 420 210 160 350 130 U 120 U 150 U 62 J 550 11,000 JDibenzo(a,h)anthracene µg/kg 160 130 U 95 J 130 U 120 U 140 U 120 U 99 J 53 J 140 U 49 J 130 U 120 U 150 U 140 UJ 76 J 1,600Dibenzofuran µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 150 JDiethylphthalate µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UDimethylphthalate µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UDi-n-butylphthalate µg/kg 140 U 130 U 51 J 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UDi-n-octylphthalate µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 180 UFluoranthene µg/kg 240 130 U 75 J 130 U 120 U 140 U 120 U 160 U 57 J 240 380 130 U 120 U 150 U 52 J 190 U 1,500Fluorene µg/kg 62 J 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 UJ 190 U 820Hexachlorobenzene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UHexachlorobutadiene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UHexachlorocyclopentadiene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UHexachloroethane µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 U

Chemical Name Result

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Table 3aOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-49-01 through OC-54-02Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, Ohio

Location ID OC-49 OC-49 OC-50 OC-50 OC-50 OC-51 OC-51 OC-52 OC-52 OC-52 OC-52 OC-52 OC-52 OC-53 OC-53 OC-54 OC-54Field Sample ID OC-49-01 OC-49-02 OC-50-01 OC-50-02 OC-50-03 OC-51-01 OC-51-02 OC-52-01 OC-52-01-DP OC-52-02 OC-52-02-DP OC-52-03 OC-52-03-DP OC-53-01 OC-53-02 OC-54-01 OC-54-02

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 0- 24 24- 48 0- 24 24- 48 48- 63 0- 24 24- 48 0- 24 0- 24 24- 48 24- 48 48- 64 48- 64 0- 24 24- 32 0- 24 24- 48

UnitChemical Name Result

Indeno(1,2,3-cd)pyrene µg/kg 100 J 130 U 63 J 130 U 120 U 140 U 120 U 55 J 140 U 69 J 140 J 130 U 120 U 150 U 140 UJ 190 U 800Isophorone µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UNaphthalene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 480Nitrobenzene µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UN-Nitroso-di-n-propylamine µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UN-Nitrosodiphenylamine µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 190 U 180 UPentachlorophenol µg/kg 230 U 220 U 250 U 220 U 200 U 250 U 210 U 270 U 240 U 240 U 230 U 220 U 210 U 250 U 240 U 320 U 310 UPhenanthrene µg/kg 640 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 110 J 200 130 U 120 U 150 U 100 J 200 8,700 JPhenol µg/kg 140 U 130 U 150 U 130 U 120 U 140 U 120 U 160 U 140 U 140 U 140 U 130 U 120 U 150 U 140 U 210 190Pyrene µg/kg 850 130 U 230 130 U 120 U 49 J 120 U 220 170 330 470 130 U 120 U 150 U 60 J 300 5,900 JTotal Parent PAHs (Sum of detections x 1.7)

µg/kg 8,568 0 U 2,950 0 U 0 U 83.3 0 U 2,671 1,566 2,559 4,860 0 U 0 U 0 U 465.8 3,014 79,968

Notes:µg/kg = Microgram per kilogramID = Identificationin. bss = Inches below sediment surface J = Analyte identification is acceptable; reported value is an estimate PAH = Polycyclic aromatic hydrocarbonSVOC = Semivolatile organic compoundU = Compound analyzed for but not detected above reported detection limiUJ = Compound analyzed for but not detected above reported estimated detection limi

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Table 3bOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-54-03 through OC-58-02Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, OhioLocation ID OC-54 OC-55 OC-55 OC-56 OC-56 OC-56 OC-56 OC-56 OC-57 OC-57 OC-57 OC-57 OC-57 OC-58 OC-58

Field Sample ID OC-54-03 OC-55-01 OC-55-02 OC-56-01 OC-56-02 OC-56-03 OC-56-04 OC-56-05 OC-57-01 OC-57-02 OC-57-03 OC-57-04 OC-57-05 OC-58-01 OC-58-02Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011

Depth Interval (in. bss) 48- 65 0- 24 24- 42 0- 24 24- 48 48- 72 72- 96 96- 112 0- 24 24- 48 48- 72 72- 96 96- 112 0- 24 24- 48Unit

1,1'-Biphenyl µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U1,2,4,5-Tetrachlorobenzene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,2'-Oxybis(1-chloropropane) µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,3,4,6-Tetrachlorophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,4,5-Trichlorophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,4,6-Trichlorophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,4-Dichlorophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,4-Dimethylphenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,4-Dinitrophenol µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 U2,4-Dinitrotoluene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2,6-Dinitrotoluene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2-Chloronaphthalene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2-Chlorophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2-Methylnaphthalene µg/kg 390 160 U 150 U 110 J 200 240 100 J 49 J 67 J 740 2,400 1,600 2,500 180 U 150 U2-Methylphenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U2-Nitroaniline µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 U2-Nitrophenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U3,3'-Dichlorobenzidine µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U3-Nitroaniline µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 U4,6-Dinitro-2-methylphenol µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 U4-Bromophenyl-phenylether µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U4-Chloro-3-methylphenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U4-Chloroaniline µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U4-Chlorophenyl-phenylether µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 U4-Methylphenol µg/kg 250 160 U 150 U 270 72 J 100 J 58 J 130 U 210 300 320 280 320 180 U 150 U4-Nitroaniline µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 U4-Nitrophenol µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 UAcenaphthene µg/kg 220 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 92 J 190 U 98 J 160 U 180 U 150 UAcenaphthylene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UAcetophenone µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UAnthracene µg/kg 890 160 U 150 U 170 U 150 110 J 60 J 130 U 170 U 260 210 190 U 180 180 U 150 UAtrazine µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UBenzaldehyde µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UBenzo(a)anthracene µg/kg 3,300 130 J 150 U 330 450 J 400 250 130 J 69 J 1,200 660 190 J 370 180 U 150 JBenzo(a)pyrene µg/kg 2,300 110 J 150 U 260 290 340 160 95 J 64 J 870 490 160 J 380 180 U 110 JBenzo(b)fluoranthene µg/kg 1,600 120 J 150 U 250 220 250 140 83 J 59 J 840 320 110 J 310 180 U 77 JBenzo(g,h,i)perylene µg/kg 1,500 72 J 150 U 200 180 240 110 J 65 J 170 U 700 420 120 J 300 180 U 74 JBenzo(k)fluoranthene µg/kg 1,200 160 U 150 U 170 U 120 J 110 J 71 J 130 U 170 U 370 190 J 190 U 100 J 180 U 150 UBis(2-chloroethoxy)methane µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UBis(2-chloroethyl)ether µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UBis(2-ethylhexyl)phthalate µg/kg 210 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UButylbenzylphthalate µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UCaprolactam µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UCarbazole µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UChrysene µg/kg 7,400 J 110 J 150 U 840 560 J 820 440 310 200 3,500 820 210 J 560 180 U 260Dibenzo(a,h)anthracene µg/kg 1,100 160 U 150 U 130 J 170 200 100 J 49 J 170 U 490 350 110 J 260 180 U 150 UDibenzofuran µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UDiethylphthalate µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UDimethylphthalate µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UDi-n-butylphthalate µg/kg 160 U 160 U 91 J 170 U 130 U 55 J 130 U 830 170 U 200 U 190 U 190 U 160 U 180 U 150 U

Chemical Name Result

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Table 3bOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-54-03 through OC-58-02Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, OhioLocation ID OC-54 OC-55 OC-55 OC-56 OC-56 OC-56 OC-56 OC-56 OC-57 OC-57 OC-57 OC-57 OC-57 OC-58 OC-58

Field Sample ID OC-54-03 OC-55-01 OC-55-02 OC-56-01 OC-56-02 OC-56-03 OC-56-04 OC-56-05 OC-57-01 OC-57-02 OC-57-03 OC-57-04 OC-57-05 OC-58-01 OC-58-02Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011

Depth Interval (in. bss) 48- 65 0- 24 24- 42 0- 24 24- 48 48- 72 72- 96 96- 112 0- 24 24- 48 48- 72 72- 96 96- 112 0- 24 24- 48UnitChemical Name Result

Di-n-octylphthalate µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UFluoranthene µg/kg 1,700 190 150 U 180 180 J 160 84 J 55 J 170 U 580 190 190 UJ 220 180 U 150 UFluorene µg/kg 800 160 U 150 U 170 U 170 140 J 73 J 52 J 170 U 280 350 140 J 320 180 U 150 UHexachlorobenzene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UHexachlorobutadiene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UHexachlorocyclopentadiene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UHexachloroethane µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UIndeno(1,2,3-cd)pyrene µg/kg 580 62 J 150 U 79 J 100 J 110 J 54 J 130 U 170 U 260 190 190 U 180 180 U 150 UIsophorone µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UNaphthalene µg/kg 160 U 160 U 150 U 71 J 120 J 89 J 130 U 130 U 170 U 130 J 350 260 420 180 U 150 UNitrobenzene µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UN-Nitroso-di-n-propylamine µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UN-Nitrosodiphenylamine µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 200 U 190 U 190 U 160 U 180 U 150 UPentachlorophenol µg/kg 270 U 270 U 250 U 290 U 220 U 260 U 220 U 220 U 290 U 340 U 320 U 320 U 280 U 300 U 260 UPhenanthrene µg/kg 5,700 J 65 J 150 U 390 780 730 470 300 160 J 3,900 1,200 340 1,100 180 U 150 UPhenol µg/kg 160 U 160 U 150 U 170 U 130 U 150 U 130 U 130 U 170 U 120 J 190 U 190 U 160 U 180 U 150 UPyrene µg/kg 5,800 J 140 J 150 U 520 410 J 470 270 190 120 J 2,100 640 190 J 510 180 U 150 JTotal Parent PAHs (Sum of detections x 1.7)

µg/kg 58,616 1,698 0 U 5,712 6,970 7,495 4,049 2,343 1,256 27,730 14,926 5,998 13,107 0 U 1,396

Notes:µg/kg = Microgram per kilogramID = Identificationin. bss = Inches below sediment surface J = Analyte identification is acceptable; reported value is an estimate PAH = Polycyclic aromatic hydrocarbonSVOC = Semivolatile organic compoundU = Compound analyzed for but not detected above reported detection limitUJ = Compound analyzed for but not detected above reported estimated detection limit

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1269-2B-AUGE

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Table 3cOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-58-03 through OC-61-05Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, Ohio

Location ID OC-58 OC-58 OC-58 OC-59 OC-59 OC-59 OC-59 OC-59 OC-60 OC-60 OC-60 OC-60 OC-60 OC-61 OC-61 OC-61 OC-61 OC-61Field Sample ID OC-58-03 OC-58-04 OC-58-05 OC-59-01 OC-59-02 OC-59-03 OC-59-04 OC-59-05 OC-60-01 OC-60-02 OC-60-03 OC-60-04 OC-60-05 OC-61-01 OC-61-02 OC-61-03 OC-61-04 OC-61-05

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 122

Unit

1,1'-Biphenyl µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U1,2,4,5-Tetrachlorobenzene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,2'-Oxybis(1-chloropropane) µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,3,4,6-Tetrachlorophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,4,5-Trichlorophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,4,6-Trichlorophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,4-Dichlorophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,4-Dimethylphenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,4-Dinitrophenol µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 U2,4-Dinitrotoluene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2,6-Dinitrotoluene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2-Chloronaphthalene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2-Chlorophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2-Methylnaphthalene µg/kg 170 U 180 U 170 U 150 UJ 170 J 280 J 450 J 1,400 J 140 J 1,400 J 1,300 J 3,800 J 1,700 J 200 U 180 U 180 U 160 J 310 J2-Methylphenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U2-Nitroaniline µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 U2-Nitrophenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U3,3'-Dichlorobenzidine µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U3-Nitroaniline µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 U4,6-Dinitro-2-methylphenol µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 U4-Bromophenyl-phenylether µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U4-Chloro-3-methylphenol µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U4-Chloroaniline µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U4-Chlorophenyl-phenylether µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U4-Methylphenol µg/kg 170 U 180 U 170 U 150 U 200 170 150 J 480 360 640 260 250 410 100 J 89 J 90 J 370 4904-Nitroaniline µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 U4-Nitrophenol µg/kg 290 U 310 U 290 U 250 UJ 280 UJ 270 UJ 300 UJ 290 UJ 310 UJ 310 UJ 310 UJ 300 UJ 320 UJ 340 U 300 U 310 U 300 UJ 310 UJAcenaphthene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 110 J 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UAcenaphthylene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 84 J 200 U 180 U 180 U 180 U 180 UAcetophenone µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UAnthracene µg/kg 170 U 180 U 170 U 150 U 170 U 81 J 170 U 77 J 180 U 250 350 370 140 J 200 U 180 U 180 U 180 U 120 JAtrazine µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UBenzaldehyde µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UBenzo(a)anthracene µg/kg 170 U 180 U 170 U 150 U 250 430 100 J 100 J 200 1,300 1,400 1,300 330 84 J 62 J 64 J 300 580Benzo(a)pyrene µg/kg 170 U 180 U 170 U 150 U 160 J 300 92 J 110 J 210 840 890 850 250 90 J 180 U 180 U 270 470Benzo(b)fluoranthene µg/kg 170 U 180 U 170 U 150 U 160 J 290 65 J 87 J 240 890 590 460 170 J 83 J 180 U 62 J 210 460Benzo(g,h,i)perylene µg/kg 170 U 180 U 170 U 150 U 130 J 230 67 J 110 J 200 670 640 640 200 86 J 180 U 180 U 220 360Benzo(k)fluoranthene µg/kg 170 U 180 U 170 U 150 U 92 J 73 J 170 U 170 U 180 U 220 640 460 75 J 200 U 180 U 180 U 240 100 JBis(2-chloroethoxy)methane µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UBis(2-chloroethyl)ether µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UBis(2-ethylhexyl)phthalate µg/kg 170 U 180 U 170 U 150 U 94 J 110 J 170 U 110 J 85 J 150 J 120 J 140 J 200 200 U 180 U 180 U 150 J 260Butylbenzylphthalate µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UCaprolactam µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UCarbazole µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 110 J 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UChrysene µg/kg 170 U 180 U 170 U 150 U 550 1,100 110 J 150 J 590 3,100 3,800 2,000 350 140 J 120 J 150 J 1,100 1,600Dibenzo(a,h)anthracene µg/kg 170 U 180 U 170 U 150 U 80 J 190 61 J 94 J 110 J 490 490 570 150 J 200 U 180 U 180 U 130 J 260Dibenzofuran µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 75 J 76 J 150 J 190 U 200 U 180 U 180 U 180 U 180 UDiethylphthalate µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UDimethylphthalate µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UDi-n-butylphthalate µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 65 J 210 200 U 70 J 180 U 180 U 660Di-n-octylphthalate µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UFluoranthene µg/kg 170 U 180 U 170 U 150 U 100 J 200 170 U 66 J 150 J 660 740 380 150 J 96 J 64 J 180 U 170 J 280Fluorene µg/kg 170 U 180 U 170 U 150 U 67 J 98 J 63 J 150 J 180 U 320 340 420 210 200 U 180 U 180 U 62 J 170 JHexachlorobenzene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UHexachlorobutadiene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UHexachlorocyclopentadiene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UHexachloroethane µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UIndeno(1,2,3-cd)pyrene µg/kg 170 U 180 U 170 U 150 U 170 U 100 J 170 U 170 U 83 J 260 250 310 110 J 200 U 180 U 180 U 72 J 150 JIsophorone µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UNaphthalene µg/kg 170 U 180 U 170 U 150 U 84 J 79 J 170 U 170 75 J 290 110 J 200 180 J 85 J 180 U 63 J 91 J 150 JNitrobenzene µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 U

Chemical Name Result

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Table 3cOctober 2011 Sampling Data - SVOC Results for Sediment Samples,

OC-58-03 through OC-61-05Duck and Otter Creeks Confluence Investigation

Toledo, Lucas County, Ohio

Location ID OC-58 OC-58 OC-58 OC-59 OC-59 OC-59 OC-59 OC-59 OC-60 OC-60 OC-60 OC-60 OC-60 OC-61 OC-61 OC-61 OC-61 OC-61Field Sample ID OC-58-03 OC-58-04 OC-58-05 OC-59-01 OC-59-02 OC-59-03 OC-59-04 OC-59-05 OC-60-01 OC-60-02 OC-60-03 OC-60-04 OC-60-05 OC-61-01 OC-61-02 OC-61-03 OC-61-04 OC-61-05

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 121 0- 24 24- 48 48- 72 72- 96 96- 122

UnitChemical Name Result

N-Nitroso-di-n-propylamine µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UN-Nitrosodiphenylamine µg/kg 170 U 180 U 170 U 150 U 170 U 160 U 170 U 170 U 180 U 180 U 180 U 180 U 190 U 200 U 180 U 180 U 180 U 180 UPentachlorophenol µg/kg 290 U 310 U 290 U 250 U 280 U 270 U 300 U 290 U 310 U 310 U 310 U 300 U 320 U 340 U 300 U 310 U 300 U 310 UPhenanthrene µg/kg 170 U 180 U 170 U 150 U 460 1,000 160 J 360 330 4,300 6,200 2,900 680 110 J 200 140 J 610 1,500Phenol µg/kg 170 U 180 U 170 U 150 U 68 J 160 U 170 U 96 J 74 J 130 J 78 J 180 U 84 J 200 U 180 U 180 U 80 J 110 JPyrene µg/kg 170 U 180 U 170 U 150 U 340 610 96 J 140 J 350 2,100 2,300 1,500 370 110 J 120 J 110 J 540 940Total Parent PAHs (Sum of detections x 1.7)

µg/kg 0 U 0 U 0 U 0 U 4,493 8,604 2,149 5,124 4,553 29,240 34,068 27,472 8,753 1,503 962.2 1,001 7,098 12,665

Notes:µg/kg = Microgram per kilogramID = Identificationin. bss = Inches below sediment surface J = Analyte identification is acceptable; reported value is an estimatePAH = Polycyclic aromatic hydrocarbonSVOC = Semivolatile organic compoundU = Compound analyzed for but not detected above reported detection limiUJ = Compound analyzed for but not detected above reported estimated detection limi

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Table 4October 2011 Sampling Data - TOC Results for Sediment Samples

Duck and Otter Creeks Confluence InvestigationToledo, Lucas County, Ohio

Location ID OC-49 OC-49 OC-49 OC-50 OC-50 OC-50 OC-50 OC-50 OC-51 OC-51 OC-51 OC-52 OC-52 OC-52 OC-52Field Sample ID OC-49 OC-49-01 OC-49-02 OC-50 OC-50-01 OC-50-02 OC-50-03 OC-50-DP OC-51 OC-51-01 OC-51-02 OC-52 OC-52-01 OC-52-01-DP OC-52-02

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 0- 6 0- 24 24- 48 0- 6 0- 24 24- 48 48- 63 0- 6 0- 6 0- 24 24- 48 0- 6 0- 24 0- 24 24- 48

UnitTOC % 3.54 1.52 0.89 3.02 3.15 0.853 0.926 3.08 2 1.38 0.583 6.25 4.37 4.37 1.98 1.98 3.39 3.39

Location ID OC-52 OC-52 OC-52 OC-53 OC-53 OC-53 OC-54 OC-54 OC-54 OC-54 OC-55 OC-55 OC-55 OC-56 OC-56Field Sample ID OC-52-02-DP OC-52-03 OC-52-03-DP OC-53 OC-53-01 OC-53-02 OC-54 OC-54-01 OC-54-02 OC-54-03 OC-55 OC-55-01 OC-55-02 OC-56 OC-56-01

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 24- 48 48- 64 48- 64 0- 6 0- 24 24- 32 0- 6 0- 24 24- 48 48- 65 0- 6 0- 24 24- 42 0- 6 0- 24

UnitTOC % 1.81 1.81 0.714 0.714 2.28 2.28 2.02 1.23 1.14 2.94 3.37 4.27 3.85 2.05 1.54 2.92 3.69 3.71

Location ID OC-56 OC-56 OC-56 OC-56 OC-57 OC-57 OC-57 OC-57 OC-57 OC-57 OC-58 OC-58 OC-58 OC-58 OC-58Field Sample ID OC-56-02 OC-56-03 OC-56-04 OC-56-05 OC-57 OC-57-01 OC-57-02 OC-57-03 OC-57-04 OC-57-05 OC-58 OC-58-01 OC-58-02 OC-58-03 OC-58-04

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 24- 48 48- 72 72- 96 96- 112 0- 6 0- 24 24- 48 48- 72 72- 96 96- 112 0- 6 0- 24 24- 48 48- 72 72- 96

UnitTOC % 2.64 1.66 2.87 1.63 4.35 2.86 4.76 4.91 4.03 3.17 2.43 2.99 2.69 3.48 2.92

Location ID OC-58 OC-59 OC-59 OC-59 OC-59 OC-59 OC-59 OC-60 OC-60 OC-60 OC-60 OC-60 OC-60 OC-61 OC-61Field Sample ID OC-58-05 OC-59 OC-59-01 OC-59-02 OC-59-03 OC-59-04 OC-59-05 OC-60 OC-60-01 OC-60-02 OC-60-03 OC-60-04 OC-60-05 OC-61 OC-61-01

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 96- 121 0- 6 0- 24 24- 48 48- 72 72- 96 96- 121 0- 6 0- 24 24- 48 48- 72 72- 96 96- 121 0- 6 0- 24

UnitTOC % 2.79 2.81 2.78 2.53 3.37 4.41 3.87 5.59 4.29 4.89 6.16 6.06 5.16 2.53 2.58

Location ID OC-61 OC-61 OC-61 OC-61Field Sample ID OC-61-02 OC-61-03 OC-61-04 OC-61-05

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 24- 48 48- 72 72- 96 96- 122

UnitTOC % 2.58 3.28 3.55 3.94

Notes:% = PercentDP = DuplicateID = Identificationin. bss = Inches below sediment surface TOC = Total organic carbonAll samples analyzed using United States Environmental Protection Agency Method SW9606M.

Chemical Name

Chemical Name Result

Result

Chemical Name

Chemical Name

Chemical Name

Result

Result

Result

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Table 5October 2011 Sampling Data - Pore Water ResultsDuck and Otter Creeks Confluence Investigation

Toledo, Lucas County, Ohio

Location ID OC-49 OC-50 OC-50 OC-51 OC-52 OC-53 OC-54 OC-55 OC-56 OC-57 OC-58 OC-59 OC-60 OC-61Field Sample ID OC-49_W OC-50_W OC-50-DP_W OC-51_W OC-52_W OC-53_W OC-54_W OC-55_W OC-56_W OC-57_W OC-58_W OC-59_W OC-60_W OC-61_W

Sampling Date 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011 10/18/2011Depth Interval (in. bss) 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6 0- 6

UnitE415.1 Dissolved organic carbon mg/L 10.4 13 41.7 12.8 16.4 71 15.1 11.4 47.3 111 13 39.2 63.1 50.1PAH34 1-Methylnaphthalene ng/g 0.22 J 0.13 J NA 0.05 U 0.22 J 0.05 U 0.05 U 0.05 U 0.88 J 0.05 U 0.05 U 0.05 U 0.05 U 0.05 UPAH34 2-Methylnaphthalene ng/g 0.09 J 0.12 J NA 0.05 U 0.08 J 0.05 U 0.05 U 0.05 U 0.08 J 0.05 U 0.05 U 0.05 U 0.05 U 0.05 UPAH34 Acenaphthene ng/g 0.67 J 1.06 NA 0.13 J 0.67 J 0.1 U 0.1 U 0.1 U 0.72 J 0.13 J 0.1 U 0.1 U 0.13 J 0.1 UPAH34 Acenaphthylene ng/g 0.36 J 0.53 J NA 0.2 U 0.37 J 0.2 U 0.2 U 0.2 U 0.44 J 0.2 U 0.2 U 0.2 U 0.2 U 0.2 UPAH34 Anthracene ng/g 0.89 1.87 NA 0.09 J 0.71 0.05 U 0.05 U 0.05 U 1.02 0.05 U 0.05 U 0.05 U 0.05 J 0.05 UPAH34 Benzo(a)anthracene ng/g 0.73 2.12 NA 0.04 J 1 0.01 J 0.03 J 0.001 U 0.53 0.02 J 0.001 U 0.001 U 0.03 J 0.004 JPAH34 Benzo(a)pyrene ng/g 0.13 0.72 NA 0.008 U 0.32 0.008 U 0.008 U 0.008 U 0.14 0.008 U 0.008 U 0.008 U 0.008 U 0.008 UPAH34 Benzo(e)pyrene ng/g 0.2 0.005 U NA 0.005 U 0.36 0.005 U 0.005 U 0.005 U 0.18 0.005 U 0.005 U 0.005 U 0.005 U 0.005 UPAH34 Benzo(g,h,i)perylene ng/g 0.009 J 0.01 J NA 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 UPAH34 Benzo[b+k]fluoranthene ng/g 0.09 0.31 NA 0.005 U 0.18 0.005 U 0.005 U 0.005 U 0.12 J 0.005 U 0.005 U 0.005 U 0.005 U 0.005 UPAH34 C1 Chrysenes ng/g 0.85 4.48 E NA 0.06 J 1.78 E 0.07 J 0.11 J 0.02 J 0.38 0.09 J 0.005 U 0.005 U 0.11 J 0.005 UPAH34 C1-Fluoranthenes/Pyrenes ng/g 5.49 16.22 NA 0.44 J 4.82 0.28 J 0.47 J 0.06 J 5.97 0.53 0.01 U 0.01 U 0.45 J 0.01 UPAH34 C1-Fluorenes ng/g 8.7 9.18 NA 0.83 J 4.53 0.38 J 0.45 J 0.19 J 8.36 0.54 J 0.02 U 0.02 U 0.59 J 0.02 UPAH34 C1-Phenanthrenes/Anthracenes ng/g 22.64 5.61 NA 0.54 J 4.64 0.34 J 0.54 J 0.11 J 19.03 0.48 J 0.02 U 0.02 U 0.93 J 0.02 UPAH34 C2 Chrysenes ng/g 0.73 5.8 E NA 0.01 U 2.38 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 UPAH34 C2-Fluorenes ng/g 10.53 18.28 NA 1.37 7.13 0.66 J 1.02 J 0.05 U 11.7 1.17 J 0.05 U 0.05 U 1.1 J 0.05 UPAH34 C2-Naphthalenes ng/g 6.7 3.55 NA 0.87 J 6.79 0.75 J 0.7 J 0.57 J 22.17 0.71 J 0.15 U 0.32 J 1.79 J 0.15 UPAH34 C2-Phenanthrenes/Anthracenes ng/g 23.67 23.43 NA 1.94 J 12.87 1.62 J 2.37 J 0.34 J 25.72 2.4 J 0.05 U 0.05 U 2.41 J 0.05 UPAH34 C3 Chrysenes ng/g 0.01 U 0.01 U NA 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 UPAH34 C3-Fluorenes ng/g 9.45 30.57 NA 0.06 U 9.4 0.06 U 0.06 U 0.06 U 16.25 4.37 0.06 U 0.06 U 0.06 U 0.06 UPAH34 C3-Naphthalenes ng/g 99.35 37 NA 7.65 60.42 3.77 J 4.57 J 1.97 J 103.3 4.09 J 0.05 U 0.25 J 9.21 0.05 UPAH34 C3-Phenanthrenes/Anthracenes ng/g 7.28 25.96 NA 1.03 J 8.22 1.05 J 1.68 J 0.33 J 13.09 1.98 J 0.04 U 0.04 U 1.23 J 0.04 UPAH34 C4 Chrysenes ng/g 0.01 U 0.01 U NA 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 U 0.01 UPAH34 C4-Naphthalenes ng/g 82.27 95.07 NA 9.06 67.9 2.14 J 6.8 J 0.26 J 52.38 2.5 J 0.15 U 0.15 U 3.48 J 0.15 UPAH34 C4-Phenanthrenes/Anthracenes ng/g 4.57 J 18.37 NA 0.02 U 4.04 J 0.02 U 1.47 J 0.02 U 6.68 J 1.29 J 0.02 U 0.02 U 0.72 J 0.02 UPAH34 Chrysene ng/g 1.25 E 2.57 E NA 0.06 J 1.54 E 0.07 0.08 0.001 U 0.62 0.07 0.001 U 0.001 U 0.11 0.006 JPAH34 Dibenzo(a,h)pyrene ng/g 0.002 U 0.002 U NA 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 U 0.002 UPAH34 Fluoranthene ng/g 1.31 1.4 NA 0.13 J 0.64 0.05 J 0.07 J 0.02 J 0.63 0.06 J 0.01 J 0.02 J 0.1 J 0.02 JPAH34 Fluorene ng/g 2.13 0.49 J NA 0.08 J 0.99 0.04 U 0.04 U 0.04 U 1.29 0.04 J 0.04 U 0.04 U 0.1 J 0.04 UPAH34 Indeno(1,2,3-cd)pyrene ng/g 0.001 U 0.005 NA 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 U 0.001 UPAH34 Naphthalene ng/g 0.62 J 0.69 J NA 0.1 J 0.7 J 0.1 U 0.1 U 0.1 U 0.48 J 0.1 J 0.1 U 0.1 U 0.1 U 1.44 JPAH34 Perylene ng/g 0.004 U 0.07 NA 0.004 U 0.07 0.004 U 0.004 U 0.004 U 0.004 U 0.004 U 0.004 U 0.004 U 0.004 U 0.004 UPAH34 Phenanthrene ng/g 6.3 0.3 J NA 0.1 U 0.21 J 0.1 U 0.1 U 0.1 U 4.5 0.1 U 0.1 U 0.1 U 0.19 J 0.1 UPAH34 Pyrene ng/g 4.57 5.07 NA 0.32 1.94 0.16 J 0.21 J 0.02 J 2.19 0.19 J 0.02 J 0.02 J 0.27 0.02 JSM4500HB pH pH units 8.32 8.23 8.4 8.32 8.49 8.25 8.43 8.17 8.17 8.18 8.26 8.18 8.16 8.02SM4500NH3E Nitrogen, Ammonia (AS N) mg/L 2.1 3.1 2.24 2.46 3.8 2.96 8.38 8.62 7.6 10.2 8.58 7.38 17.2 12.5Notes:DP = DuplicateE = Exceeded laboratory upper calibration range�ID = Identificationin. bss = Inches below sediment surface J = Analyte identification is acceptable; reported value is an estimate mg/L = Milligram per liter NA = Not applicableng/g = Nanogram per gramPAH = Polycyclic aromatic hydrocarbon U = Compound analyzed for but not detected above reported detection limit

Analytical Method Chemical Name Result

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Table 6October 2011 Sampling Data - Toxicity Testing Results

Duck and Otter Creeks Confluence InvestigationToledo, Lucas County, Ohio

Mean SD SEM CV % Control Min Max n Mean SD SEM CV % Control n Mean SD SEM CV % Control nControl 93.8% 9.2% 3.2% 9.8% 100.0% 80.0% 100.0% 8 1.317 0.179 0.063 13.6% 100.0% 8 1.431 0.330 0.117 23.1% 100.0% 8OC-49 41.3% 30.0% 10.6% 72.7% 44.0% 0.0% 80.0% 8 0.110 0.087 0.031 78.4% 8.4% 8 0.277 0.091 0.034 32.9% 19.3% 7OC-50 47.5% 14.9% 5.3% 31.3% 50.7% 30.0% 70.0% 8 0.138 0.112 0.040 81.3% 10.5% 8 0.283 0.153 0.054 54.0% 19.8% 8OC-51 78.8% 34.4% 12.2% 43.7% 84.0% 0.0% 100.0% 8 0.877 0.378 0.134 43.1% 66.6% 8 1.146 0.279 0.106 24.4% 80.1% 7OC-52 40.0% 31.2% 11.0% 77.9% 42.7% 0.0% 90.0% 8 0.122 0.136 0.048 111.8% 9.2% 8 0.291 0.133 0.050 45.8% 20.3% 7OC-53 92.5% 10.4% 3.7% 11.2% 98.7% 70.0% 100.0% 8 1.211 0.224 0.079 18.5% 91.9% 8 1.318 0.248 0.088 18.8% 92.1% 8OC-54 97.5% 4.6% 1.6% 4.7% 104.0% 90.0% 100.0% 8 1.237 0.159 0.056 12.9% 93.9% 8 1.270 0.156 0.055 12.3% 88.7% 8OC-55 92.5% 8.9% 3.1% 9.6% 98.7% 80.0% 100.0% 8 1.228 0.184 0.065 15.0% 93.2% 8 1.328 0.154 0.054 11.6% 92.8% 8OC-56 93.8% 7.4% 2.6% 7.9% 100.0% 80.0% 100.0% 8 1.200 0.113 0.040 9.5% 91.1% 8 1.286 0.149 0.053 11.6% 89.8% 8OC-57 90.0% 10.7% 3.8% 11.9% 96.0% 70.0% 100.0% 8 1.121 0.215 0.076 19.2% 85.1% 8 1.245 0.178 0.063 14.3% 87.0% 8OC-58 96.3% 7.4% 2.6% 7.7% 102.7% 80.0% 100.0% 8 1.250 0.128 0.045 10.2% 94.9% 8 1.308 0.191 0.067 14.6% 91.4% 8OC-59 91.3% 8.3% 3.0% 9.1% 97.3% 80.0% 100.0% 8 1.225 0.173 0.061 14.1% 93.0% 8 1.356 0.238 0.084 17.6% 94.7% 8OC-60 91.3% 13.6% 4.8% 14.9% 97.3% 60.0% 100.0% 8 1.268 0.214 0.076 16.9% 96.2% 8 1.421 0.329 0.116 23.1% 99.3% 8OC-61 95.0% 7.6% 2.7% 8.0% 101.3% 80.0% 100.0% 8 1.370 0.115 0.040 8.4% 104.0% 8 1.452 0.187 0.066 12.9% 101.5% 8

ID - Identification

mg - Milligramn - NumberSEM - Standard error of meanSD - Standard deviation

% - PercentCV - Control valued - Day

Max - MaximumMin - Minimum

10-d Survival (%) 10-d Individual Ash-free Dry Weight (mg)10-d Total Ash-free Biomass/Initial Organism (mg)

Sediment ID

Significantly different from control

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This document shall not be disclosed without the express written permission of U.S. EPA 1269-2B-AUGE

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ATTACHMENT C PHOTOGRAPHIC LOG

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Site: Duck and Otter Creeks Confluences Photo Number: 1 Date: 10/18/11 Direction: South Photographer: Brenda Jones Subject: View of mouth of Otter Creek from the confluence area

Site: Duck and Otter Creeks Confluences Photo Number: 2 Date: 10/18/11 Direction: Down Photographer: Brenda Jones Subject: View of surface sediment collected from location OC-56

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Site: Duck and Otter Creeks Confluences Photo Number: 3 Date: 10/18/11 Direction: Down Photographer: Brenda Jones Subject: View of surface sediment collected from location OC-60

Site: Duck and Otter Creeks Confluences Photo Number: 4 Date: 10/18/11 Direction: Down Photographer: Brenda Jones Subject: Closer view of surface sediment collected from location OC-60; note staining and sheen on water in the courser sediment

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Site: Duck and Otter Creeks Confluences Photo Number: 5 Date: 10/19/11 Direction: Down Photographer: Hilary Verduce Subject: View of sediment inside core from location OC-56

Site: Duck and Otter Creeks Confluences Photo Number: 6 Date: 10/19/11 Direction: Down Photographer: Hilary Verduce Subject: View of sediment inside core location OC-60; note greasy appearance on left side

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Site: Duck and Otter Creeks Confluences Photo Number: 7 Date: 10/17/11 Direction: Down Photographer: Brenda Jones Subject: Staining in surface sediment collected for location OC-52

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ATTACHMENT D FINAL TOXICITY TESTING REPORT

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Acute Toxicity Evaluation of Duck and

Otter Creek Sediments with Chironomus

dilutus (Confluence Site Investigation Part

3) Prepared for: Brenda Jones

U.S. EPA Great Lakes National Program Office

77 West Jackson Blvd.

Chicago, IL 60604

Prepared by: J. Daniel Farrar Burton Suedel

Department of the Army US Army Engineer Research and Development Center Environmental Laboratory 3909 Halls Ferry Rd, EP-R Vicksburg, MS 39180

8 March 2012

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ACUTE TOXICITY EVALUATION OF DUCK AND OTTER CREEK SEDIMENTS WITH CHIRONOMUS DILUTUS DRAFT-Do Not Distribute

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TABLE OF CONTENTS PHOTOS AND TABLES ............................................................................................................... 3

EXECUTIVE SUMMARY ............................................................................................................ 4

INTRODUCTION .......................................................................................................................... 5

TEST SEDIMENTS........................................................................................................................ 5

METHODS ..................................................................................................................................... 6

Water quality parameters ............................................................................................................ 6

Statistical analysis ....................................................................................................................... 7

RESULTS ....................................................................................................................................... 7

REFERENCES ............................................................................................................................... 8

APPENDICES ................................................................................................................................ 9

Appendix A. Photos from sediment toxicity bioassays ............................................................. 9

Appendix B. Water quality parameters for sediment bioassays .............................................. 10

Appendix C. Endpoint data for Duck and Otter Creeks Chironomus dilutus bioassay ........... 13

Appendix D. Statistical analyses for Duck and Otter Creeks Chironomus dilutus bioassay ... 17

Duck and Otter Creek 10-d Percent Survival ........................................................................... 17

Duck and Otter Creek 10-d Ash-free Biomass/Initial Organism .............................................. 18

Duck and Otter Creek 10-d Individual Ash-free Dry Weight/Surviving Organism ................. 19

Appendix E. Chain of Custody sheets ..................................................................................... 20

Appendix F. Laboratory data Sheets for Duck and Otter Creeks Chironomus dilutus bioassay................................................................................................................................................... 24

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PHOTOS AND TABLES Table 1. Summary of the test sediments and sediment identification. ............................................ 5 Table 2. Chironomus dilutus initial individual dry weight. ............................................................ 8 Table 3. Chironomus dilutus mean survival and mass. .................................................................. 8 Table B1. Chironomus dilutus 10-d bioassay overlying water quality parameters……………... 10 Table B2. Pore water ammonia concentrations………………………………………………..... 12 Photo A1. Zumwalt/Brunson water delivery system used during sediment toxicity bioassay testing. ............................................................................................................................................. 9 Photo A2. Close-up photo of exposure chambers used during bioassay testing. ........................... 9

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EXECUTIVE SUMMARY The Great Lakes National Program Office (GLNPO) requested the US Army Engineer Research and Development Center (ERDC) to conduct acute toxicity testing on sediments from Duck and Otter Creeks as part of its Great Lakes Legacy Act initiative. Thirteen (13) sediments from Otter Creek were evaluated using the midge Chironomus dilutus. This report summarizes the biological testing of sediment collected from Duck and Otter Creeks confluence sites conducted in basic accordance with guidance provided in “Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated Contaminants with Freshwater Invertebrates” (USEPA 2000). A significant reduction in survival and ash-free dry weight per surviving organism were detected in OC-49, OC-50 and OC-52 sediment samples (Table 3). Significant reductions in total biomass per initial organism were detected for sediment samples OC-49, OC-50, OC-51 and OC-52. No significant effects on survival or biomass/weight were detected for the remaining sediment samples evaluated.

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INTRODUCTION At the request of the USEPA Great Lakes National Program Office (GLNPO), the US Army Engineer Research and Development Center (ERDC) conducted sediment toxicity tests of bottom sediment collected from the Duck and Otter Creek confluence site. This study represents the third phase of sediment testing at the confluence site with initial testing occurring in November and December of 2010 and the second phase of testing occurring in September 2011. Duck and Otter Creeks are located in an industrialized area of Northwest Ohio. The creeks are part of the Maumee River watershed which empties into Lake Erie. The evaluations were conducted under the Great Lakes Legacy Act with support from the GLNPO. The evaluation consisted of a whole sediment acute toxicity test with the midge Chironomus dilutus. The study was conducted in basic accordance with the guidance provided in “Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated Contaminants with Freshwater Invertebrates” (USEPA 2000).

TEST SEDIMENTS Thirteen (13) sediments were received by the ERDC. All sediments were received 20 October 2011. Sediments were immediately inspected, logged and placed in cold storage at 4°C where they remained until test initiation. Chain of custody sheets are provided in Appendix D. A list of sediment samples evaluated is provided in Table 1.

Table 1. Summary of the test sediments and sediment identification.

Sample Name Customer ID

OC-49 OC-49 OC-50 OC-50 OC-51 OC-51 OC-52 OC-52 OC-53 OC-53 OC-54 OC-54 OC-55 OC-55 OC-56 OC-56 OC-57 OC-57 OC-58 OC-58 OC-59 OC-59 OC-60 OC-60 OC-61 OC-61

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METHODS Chironomus dilutus 10-day sediment exposures were conducted in basic accordance with guidance provided in “Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated Contaminants with Freshwater Invertebrates” (USEPA 2000). Testing was conducted October 31st – November 10th 2011. Egg masses were obtained from Environmental Consulting and Testing (Superior, WI) and maintained in culture until the correct age (~ 10 days old) organisms were obtained to initiate testing. On test day -3 approximately 75 mL of each sediment was added to eight (8) replicate 300 mL beakers (Appendix A; Photo A2). Sediment from the University of Mississippi field station, (Oxford, MS) was included as a negative control. Overlying water (dechlorinated Vicksburg municipal water system) was added and beakers were placed in a temperature controlled environmental chamber at 23 °C and allowed to equilibrate for two days without water exchange. Two daily water exchanges were conducted on test day -1. On test day 0, pore water ammonia measurements were taken on sediments prior to addition of organisms. Pore water was collected by centrifuging 50 mL of each sediment at 3000 RPM for 15 minutes. Pore water analysis was performed on the supernatant of the centrifuged sediment. Overlying water quality (temperature, pH, dissolved oxygen (DO), hardness, alkalinity, conductivity and ammonia) was recorded for each replicate beaker at test initiation. Ten organisms were randomly added to each replicate and 1 mL of a Tetrafin® food mixture (6 mg Tetrafin/mL) was provided. Initial dry and ash-free dry weights were determined on a subset of 20 organisms not used in testing. Initial weights of midges sampled from the pool of larvae used in testing were within the 0.08 to 0.23 mg/individual dry weight range indicative of the correct developmental stage (USEPA 2000) (Table 2). Temperature and DO were measured daily on a single replicate of each sediment throughout the exposure period. Animals were fed 1 mL of a Tetrafin® food mixture and two full water renewals were conducted daily. Water renewals were conducted using a modified Zumwalt/Brunson water renewal system (USEPA 2000) (Appendix A; Photo A1). On test day 10, overlying water quality was measured in each replicate beaker and each beaker was terminated by passing the sediment through a 425 µm screen. Surviving organisms were recovered and enumerated. Following enumeration organisms from each replicate were placed on pre-weighed pans and placed in a drying oven for 24 hours at 60 °C. Following the drying period, pans were removed from the oven and dry mass for each replicate was recorded. Pans were then placed in a muffle furnace at 550 °C for 2 hours. After 2 hours, pans were removed from the furnace allowed to cool and ash-free dry mass was recorded for each replicate.

Water quality parameters

The water quality during bioassay testing was measured using a Thermo Scientific Orion 4Star meter (Thermo Scientific, Beverly, MA) for electrical conductivity, a model 315i meter (WTW; Weilheim, Germany) for pH, and a model Oxi 330 meter (WTW; Weilheim, Germany) for DO. Total overlying water ammonia, hardness and alkalinity were measured using LeMotte titration kits (Chestertown, MD, USA). Total pore water ammonia was measured using a 720A ion-

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selective electrode (ISE) meter (Thermo Orion Electron Corp., Beverly, MA) equipped with a 95-12 ammonia-sensitive electrode (Thermo Orion Electron Corp., Beverly, MA).

Statistical analysis

Data normality (Kolmogorov–Smirnov test), homogeneity (Levene’s Test), and sediment differences compared to the control were conducted using SigmaStat software (Version 3.5, SPSS, Chicago, IL). Statistical significance was determined at α = 0.05. Survival data were arcsine-square-root transformed prior to analysis. Where data were normal and homogeneous a one-way ANOVA was conducted followed by means comparison to the control using the Dunnett’s mean comparison method. Where data were not normal and/or homogenous, the Kruskal–Wallis one-way ANOVA on ranks was applied followed by means comparison to the control using the Dunnett’s mean comparison procedure. Data endpoints analyzed include survival, ash-free biomass per initial organism, and ash-free dry weight per surviving organism.

RESULTS Water quality parameters for the Chironomus dilutus 10-day bioassay were within the acceptability ranges specified by testing guidance (US EPA 2000) (Appendix B; Table B1). All pore water total ammonia concentrations were below the 20 mg/L guidance for freshwater organisms provided in the Inland Testing Manual (USEPA /USACE 1998) (Appendix B; Table B2). Survival in the negative control was 93.8% and exceeded the 70% performance requirement indicated in testing guidance (US EPA 2000) (Table 3). The performance criterion of minimum ash-free individual control weight equaling or exceeding 0.48 mg was also met with control individual ash-free dry weight measuring 1.43 mg. Survival ranged from 40.0% to 97.5% in the sediment samples tested (Table 3). A significant reduction in survival was detected in sediment samples OC-49, OC-50 and OC-52. Significant reductions in total biomass per initial organism were detected for sediment samples OC-49, OC-50, OC-51 and OC-52 and significant reductions in ash-free dry weight per surviving organism were detected for sediment samples OC-49, OC-50 and OC-52. No significant effects on survival or biomass/weight were detected for the remaining sediment samples evaluated.

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Table 2. Chironomus dilutus initial individual dry weight. Mean dry weight (± one standard deviation).

Organism Individual Dry

Weight (mg)

Individual Ash-

free Dry Weight

(mg)

Chironomus dilutus 0.221 ± 0.05 0.067 ± 0.06 Table 3. Chironomus dilutus mean survival and mass (± one standard deviation). Asterisks denote a statistically significant reduction in survival or mass relative to the control sediment.

Sample Name % Survival

Ash-Free

Biomass/

Initial

Organism

(mg)

Ash-free Dry

Weight per

Surviving

Organism

(mg)

Control 93.8 ± 9.2 1.317 ± 0.179 1.431 ± 0.330 OC-49 41.3 ± 30.0* 0.110 ± 0.087* 0.277 ± 0.091* OC-50 47.5 ± 14.9* 0.138 ± 0.112* 0.283 ± 0.153* OC-51 78.8 ± 34.4 0.877 ± 0.378* 1.146 ± 0.279 OC-52 40.0 ± 31.2* 0.122 ± 0.136* 0.291 ± 0.133* OC-53 92.5 ± 10.4 1.211 ± 0.224 1.318 ± 0.248 OC-54 97.5 ± 4.6 1.237 ± 0.159 1.270 ± 0.156 OC-55 92.5 ± 8.9 1.228 ± 0.184 1.328 ± 0.154 OC-56 93.8 ± 7.4 1.200 ± 0.113 1.286 ± 0.149 OC-57 90.0 ± 10.7 1.121 ± 0.215 1.245 ± 0.178 OC-58 96.3 ± 7.4 1.250 ± 0.128 1.308 ± 0.191 OC-59 91.3 ± 8.3 1.225 ± 0.173 1.356 ± 0.238 OC-60 91.3 ± 13.6 1.268 ± 0.214 1.421 ± 0.329 OC-61 95.0 ± 7.6 1.370 ± 0.115 1.452 ± 0.187

REFERENCES US Environmental Protection Agency / US Army Corps of Engineers (US EPA / USACE). 1998. Evaluation of Material Proposed for Discharge to Waters of the U.S. - Testing Manual (Inland Testing Manual). EPA-823-B-98-004, Office of Water, Washington DC. US Environmental Protection Agency. 2000. Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated Contaminants with Freshwater Invertebrates, Second Edition. EPA 600/R-99/064, Office of Water, Washington, D.C.

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APPENDICES

Appendix A. Photos from sediment toxicity bioassays

Photo A1. Zumwalt/Brunson water delivery system used during sediment toxicity bioassay testing.

Photo A2. Close-up of exposure chambers used during bioassay testing.

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Appendix B. Water quality parameters for sediment bioassays

Table B1. Chironomus dilutus 10-d bioassay overlying water quality parameters. Means ± one standard deviation from the mean are indicated, with the minimum and maximum range of the data provided in parentheses. <1 indicates below detection limit.

Treatment Temperature

( C)

pH

(SU)

Dissolved oxygen

(mg/L)

Conductivity

(µS/cm)

*Maximum

Ammonia

(mg/L)

*Alkalinity

(mg/L)

*Hardness

(mg/L)

Control 23.4 ± 0.2

(23.1 - 23.9) 7.5 ± 0.1

(7.2 – 7.7) 7.2 ± 1.2

(5.0 – 8.8) 337 ± 95

(216 – 464) 3 78 ± 4 ( 75 - 80)

75 ± 0 (75 - 75)

OC-49 23.1 ± 0.1

(22.8 - 23.4) 7.7 ± 0.3

(7.3 – 8.1) 6.7 ± 0.8

(5.4 – 7.7) 298 ± 47

(202 - 362) <1 97 ± 10 (90 - 104)

78 ± 11 (70 - 85)

OC-50 23.3 ± 0.2

(23.0 - 23.6) 7.7 ± 0.3

(7.2 – 8.1) 6.6 ± 1.2

(3.5 – 7.8) 307 ± 51

(187 – 402) <1 95 ± 7 (90 - 100)

83 ± 4 (80 - 85)

OC-51 23.1 ± 0.2

(22.8 – 23.4) 7.8 ± 0.3

(7.3 – 8.2) 6.6 ± 1.1

(4.3 – 8.1) 310 ± 37

(245 - 371) <1 96 ± 23 (80 – 112)

75 ± 7 (70 - 80)

OC-52 23.3 ± 0.2

(22.8 – 23.6) 7.7 ± 0.2 (7.3 - 8.0)

6.4 ± 1.0 (4.7 – 7.5)

302 ± 48 (235 - 377) <1 103 ± 11

(95 - 110) 75 ± 7

(75 - 80)

OC-53 23.3 ± 0.1

(23.1 – 23.5) 7.8 ± 0.2

(7.5 – 8.1) 6.5 ± 1.1

(4.9 – 8.0) 315 ± 48

(254 - 380) <1 115 ± 21 (100 - 130)

78 ± 4 (75 - 80)

OC-54 23.3 ± 0.2

(23.0 – 23.5) 7.8 ± 0.3

(7.4 – 8.1) 6.6 ± 1.4

(4.3 – 7.8) 313± 32

(256 – 362) <1 104 ± 6 (100 - 108)

88 ± 11 (80 - 95)

OC-55 23.4 ± 0.2

(22.9 - 23.7) 7.8 ± 0.3

(7.3 – 8.1) 6.5 ± 1.1

(4.7 – 7.9) 305 ± 20

(276 - 343) <1 103 ± 4 (100 - 105)

83 ± 18 (70 - 95)

OC-56 23.3 ± 0.1

(23.0 – 23.4) 7.7 ± 0.2 (6.9 – 8.5)

6.5 ± 1.2 (4.8 – 8.2)

311 ± 29 (258 - 372) <1 109 ± 13

(100 - 118) 83 ± 18 (70 - 95)

OC-57 23.5 ± 0.2

(23.1 - 23.7) 7.8 ± 0.4

(7.3 – 8.3) 6.5 ± 1.7

(2.5 – 8.4) 304 ± 43

(245 – 415) <1 118 ± 11 (110 - 125)

80 ± 14 (70 - 90)

OC-58 23.3 ± 0.3

(22.4 - 23.7) 7.7 ± 0.3

(7.3 – 8.0) 6.4 ± 1.1

(4.2 – 7.8) 337 ± 46

(275 – 395) 1 114 ± 23 (98 - 130)

88 ± 11 (80 - 95)

OC-59 23.2 ± 0.2

(22.8– 23.5) 7.8 ± 0.3

(7.4 – 8.2) 7.0 ± 1.0

(5.0 – 8.5) 300 ± 34

(246 – 368) <1 95 ± 7 (90 - 100)

77 ± 10 (70 - 84)

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Treatment Temperature

( C)

pH

(SU)

Dissolved oxygen

(mg/L)

Conductivity

(µS/cm)

*Maximum

Ammonia

(mg/L)

*Alkalinity

(mg/L)

*Hardness

(mg/L)

OC-60 23.3 ± 0.2

(22.9 - 23.6) 7.7 ± 0.3

(7.2 – 8.1) 6.5 ± 1.4

(4.4 – 7.9) 318 ± 77

(237 – 570) 2 110 ± 0 (110 - 110)

93 ± 18 (80 - 105)

OC-61 23.1 ± 0.2

(22.6– 23.4) 7.7 ± 0.3

(7.2 – 8.0) 6.6 ± 1.7

(3.3 – 8.5) 349 ± 64

(210 – 429) 2 104 ± 6 (100 - 108)

89 ± 13 (80 - 98)

*Measurement taken on composite sample

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Table B2. Pore water ammonia concentrations at Chironomus dilutus 10-day test initiation. Unionized ammonia concentration predicted based on the standard test temperature of 23°C.

Treatment Total Ammonia

(mg/L)

Unionized

Ammonia

(mg/L)

pH

(SU)

OC-49 6.97 0.0411 7.08 OC-50 6.35 0.0998 7.51 OC-51 4.31 0.0440 7.32 OC-52 10.3 0.169 7.53 OC-53 6.78 0.0632 7.28

OC-54 10.5 0.0410 6.90

OC-55 13.3 0.0700 7.03

OC-56 2.42 0.0310 7.42

OC-57 2.78 0.0311 7.36

OC-58 4.05 0.0443 7.35

OC-59 2.55 0.0401 7.51

OC-60 6.37 0.0567 7.26

OC-61 2.96 0.0371 7.41

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Appendix C. Endpoint data for Duck and Otter Creeks Chironomus dilutus bioassay

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Appendix D. Statistical analyses for Duck and Otter Creeks Chironomus dilutus bioassay

Duck and Otter Creek 10-d Percent Survival One Way Analysis of Variance Thursday, December 01, 2011, 3:16:54 PM Data source: Data 1 in Notebook 1 Normality Test: Failed (P = <0.001) Test execution ended by user request, ANOVA on Ranks begun Kruskal-Wallis One Way Analysis of Variance on Ranks Thursday, December 01, 2011, 3:16:54 PM Data source: Data 1 in Notebook 1 Group N Missing Median 25% 75%

Control 8 0 1.571 1.178 1.571 OC-49 8 0 0.632 0.451 0.997 OC-50 8 0 0.735 0.632 0.886 OC-51 8 0 1.410 0.991 1.571 OC-52 8 0 0.735 0.322 0.886 OC-53 8 0 1.410 1.249 1.571 OC-54 8 0 1.571 1.410 1.571 OC-55 8 0 1.410 1.178 1.571 OC-56 8 0 1.410 1.249 1.571 OC-57 8 0 1.249 1.178 1.571 OC-58 8 0 1.571 1.410 1.571 OC-59 8 0 1.249 1.178 1.571 OC-60 8 0 1.410 1.249 1.571 OC-61 8 0 1.571 1.249 1.571 H = 57.157 with 13 degrees of freedom. (P = <0.001) The differences in the median values among the treatment groups are greater than would be expected by chance; there is a statistically significant difference (P = <0.001) To isolate the group or groups that differ from the others use a multiple comparison procedure. Multiple Comparisons versus Control Group (Dunnett's Method) : Comparison Diff of Ranks q' P<0.05

OC-50 vs Control 440.000 3.387 Yes OC-49 vs Control 438.500 3.376 Yes OC-52 vs Control 430.500 3.314 Yes OC-51 vs Control 103.500 0.797 No OC-57 vs Control 81.500 0.627 Do Not Test OC-54 vs Control 73.500 0.566 Do Not Test OC-59 vs Control 73.000 0.562 Do Not Test OC-58 vs Control 55.000 0.423 Do Not Test OC-55 vs Control 36.500 0.281 Do Not Test OC-60 vs Control 32.000 0.246 Do Not Test OC-53 vs Control 26.500 0.204 Do Not Test OC-61 vs Control 18.500 0.142 Do Not Test OC-56 vs Control 18.000 0.139 Do Not Test

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Duck and Otter Creek 10-d Ash-free Biomass/Initial Organism

One Way Analysis of Variance Thursday, December 01, 2011, 3:18:36 PM Data source: Data 1 in Notebook 1 Normality Test: Failed (P = 0.024) Test execution ended by user request, ANOVA on Ranks begun Kruskal-Wallis One Way Analysis of Variance on Ranks Thursday, December 01, 2011, 3:18:36 PM Data source: Data 1 in Notebook 1 Group N Missing Median 25% 75%

Control 8 0 1.308 1.218 1.434 OC-49 8 0 0.0840 0.0462 0.198 OC-50 8 0 0.101 0.0869 0.124 OC-51 8 0 1.002 0.821 1.088 OC-52 8 0 0.102 0.0292 0.140 OC-53 8 0 1.165 1.041 1.394 OC-54 8 0 1.216 1.176 1.329 OC-55 8 0 1.237 1.081 1.301 OC-56 8 0 1.228 1.121 1.275 OC-57 8 0 1.082 0.947 1.296 OC-58 8 0 1.250 1.146 1.339 OC-59 8 0 1.236 1.091 1.319 OC-60 8 0 1.355 1.131 1.420 OC-61 8 0 1.364 1.275 1.463 H = 68.748 with 13 degrees of freedom. (P = <0.001) The differences in the median values among the treatment groups are greater than would be expected by chance; there is a statistically significant difference (P = <0.001) To isolate the group or groups that differ from the others use a multiple comparison procedure. Multiple Comparisons versus Control Group (Dunnett's Method) : Comparison Diff of Ranks q' P<0.05

OC-49 vs Control 551.000 4.242 Yes OC-52 vs Control 550.000 4.234 Yes OC-50 vs Control 535.000 4.118 Yes OC-51 vs Control 368.000 2.833 Yes OC-57 vs Control 198.500 1.528 No OC-56 vs Control 129.000 0.993 Do Not Test OC-53 vs Control 125.000 0.962 Do Not Test OC-55 vs Control 115.000 0.885 Do Not Test OC-59 vs Control 105.000 0.808 Do Not Test OC-54 vs Control 98.000 0.754 Do Not Test OC-58 vs Control 79.000 0.608 Do Not Test OC-61 vs Control 71.500 0.550 Do Not Test OC-60 vs Control 32.000 0.246 Do Not Test

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Duck and Otter Creek 10-d Individual Ash-free Dry Weight/Surviving Organism One Way Analysis of Variance Thursday, December 01, 2011, 3:22:23 PM Data source: Data 2 in Notebook 1 Normality Test: Passed (P > 0.050) Equal Variance Test: Passed (P = 0.340) Group Name N Missing Mean Std Dev SEM

Control 8 0 1.431 0.330 0.117 OC-49 7 0 0.277 0.0911 0.0344 OC-50 8 0 0.283 0.153 0.0541 OC-51 7 0 1.146 0.279 0.106 OC-52 7 0 0.291 0.133 0.0503 OC-53 8 0 1.318 0.248 0.0877 OC-54 8 0 1.270 0.156 0.0553 OC-55 8 0 1.328 0.154 0.0545 OC-56 8 0 1.286 0.149 0.0526 OC-57 8 0 1.245 0.178 0.0631 OC-58 8 0 1.308 0.191 0.0674 OC-59 8 0 1.356 0.238 0.0843 OC-60 8 0 1.421 0.329 0.116 OC-61 8 0 1.452 0.187 0.0661 Source of Variation DF SS MS F P

Between Groups 13 19.690 1.515 33.059 <0.001 Residual 95 4.352 0.0458 Total 108 24.042 The differences in the mean values among the treatment groups are greater than would be expected by chance; there is a statistically significant difference (P = <0.001). Power of performed test with alpha = 0.050: 1.000 Multiple Comparisons versus Control Group (Dunnett's Method) : Comparisons for factor: Sediment Comparison Diff of Means q' P P<0.050

Control vs. OC-49 1.154 10.419 -- Yes Control vs. OC-50 1.148 10.723 -- Yes Control vs. OC-52 1.140 10.293 -- Yes Control vs. OC-51 0.285 2.568 -- No Control vs. OC-57 0.186 1.734 -- Do Not Test Control vs. OC-54 0.161 1.507 -- Do Not Test Control vs. OC-56 0.145 1.358 -- Do Not Test Control vs. OC-58 0.123 1.148 -- Do Not Test Control vs. OC-53 0.113 1.054 -- Do Not Test Control vs. OC-55 0.103 0.960 -- Do Not Test Control vs. OC-59 0.0753 0.704 -- Do Not Test Control vs. OC-61 0.0215 0.201 -- Do Not Test Control vs. OC-60 0.00959 0.0896 -- Do Not Test

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Appendix E. Chain of Custody sheets

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Appendix F. Laboratory data Sheets for Duck and Otter Creeks Chironomus dilutus

bioassay

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