FINAL Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Prepared for

Fish & Wildlife Compensation Program’s Peace Region 9228 – 100th Ave. Ft. St. John, BC V1J 1X7

June 2016

Azimuth Consulting Group Partnership 218-2902 West Broadway Vancouver, BC V6K 2G8

Project No. PFWCP-15a

Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

TABLE OF CONTENTS

TABLE OF CONTENTS ...... i

LIST OF TABLES ...... ii

LIST OF FIGURES ...... ii

APPENDICES...... iv

ACKNOWLEDGEMENTS ...... v

PROFESSIONAL LIABILITY STATEMENT ...... vi

EXECUTIVE SUMMARY ...... vii

1. INTRODUCTION ...... 1 1.1. Background ...... 1 1.2. Report Objectives ...... 1 2. METHODS ...... 2 2.1. Overview ...... 2 2.2. Standard Operating Procedures ...... 3 2.3. Deviations ...... 3 2.4. Laboratory Assessed Parameters ...... 3 2.4.1. Mercury and Selenium ...... 3 2.4.2. Stable Isotopes ...... 4 2.5. Data Management ...... 5 2.5.1. Fish Catch Locations, Grouping and Categorizing ...... 5 2.5.2. Data Manipulations ...... 5 2.6. Quality Assurance Quality Control ...... 6 3. RESULTS & DISCUSSION ...... 1 3.1. Rainbow trout ...... 1 3.2. Bull trout ...... 2 3.3. Kokanee ...... 3 4. REFERENCES ...... 16

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LIST OF TABLES

Table 2-1. Summary of fish catch locations and grouping for 2015 and 2006 data. 1 Table 3-1. Summary of length (mm), weight (g), condition factor, mercury (mg/kg ww), selenium (mg/kg ww) and stable nitrogen and carbon isotopes for rainbow trout and bull trout (2015) and kokanee (2006). .... 6

LIST OF FIGURES

Figure 3-1. Overview of fish capture locations...... 7 Figure 3-2. Total mercury concentration (mg/kg ww) of tissue versus fork length (mm) for individual rainbow trout caught in Thutade Lake...... 8 Figure 3-3. Total selenium concentration (mg/kg ww) of tissue versus fork length (mm) for individual rainbow trout caught in Thutade Lake...... 8 Figure 3-4. Relationship between δ15N and fish length (mm) for individual rainbow trout caught in Thutade Lake...... 9 Figure 3-5. Relationship between δ15N and δ13C for individual rainbow trout (Thutade Lake), kokanee (2006) and bull trout, Williston Reservoir. 10 Figure 3-6. Weight (g) versus length (mm) for individual bull trout caught in tributaries of Williston Reservoir...... 11 Figure 3-7. Relationship between total mercury concentration (mg/kg ww) and fork length (mm) for individual bull trout caught in Williston Reservoir tributaries...... 11 Figure 3-8. Total selenium concentration (mg/kg ww) versus fish length mm) for individual bull trout caught in tributaries of Williston Reservoir...... 12 Figure 3-9. Relationship between δ15N and fish length (mm) for individual bull trout caught in tributaries of Williston Reservoir...... 12 Figure 3-10. Distribution of 2006 fish length data for kokanee among areas. 13 Figure 3-11. Weight versus length for individual kokanee caught in tributaries of Williston Reservoir...... 13

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Figure 3-12. Relationship between total mercury concentration (mg/kg ww) and fork length for individual kokanee in tributaries of Williston Reservoir, 2006...... 14 Figure 3-13. Relationship between total selenium concentration (mg/kg ww) and fork length for individual kokanee in tributaries of Williston Reservoir, 2006...... 14 Figure 3-14. Relationship between δ15N and fish length (mm) for individual kokanee caught in tributaries of Williston Reservoir, 2006...... 15

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APPENDICES

Appendix A. Standard Operating Procedure. Appendix B. Raw individual fish data from laboratory reports (ALS and SINLAB). Appendix C. Kokanee field photos highlighting range in morphology.

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ACKNOWLEDGEMENTS

This report was written by Laura Bekar and Randy Baker with review by Gary Mann, all of Azimuth Consulting Group Partnership (Azimuth), Vancouver BC. Maggie McConnell of Azimuth was instrumental for organizing the fish sampling phase of the Project. Key to this program were those who provided fish samples for laboratory analyses. These people included John Hagen, Ian Spendlow, Mike Tilson, Doris Jacks, Benita Kaytor, Sean Rapai, Sheila Pierre, Jimmy Were, and possibly others. A special thank you to Arne Langston and Randy Zemlak of BC Hydro for sharing their knowledge of regional fish ecology and advising on the location of sampling areas. In particular, we would like to acknowledge the leadership and guidance provided by Dan Bouillon, the Fish & Wildlife Compensation Program’s Peace Region Manager, and the FWCP’s Peace Region Board. Their participation in this project is much appreciated.

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PROFESSIONAL LIABILITY STATEMENT

This report has been prepared by Azimuth Consulting Group Partnership (‘Azimuth’) for the use of the Fish & Wildlife Compensation Program (the ‘Client’). The Client has been party to development of terms of reference for the scope of work and understands its limitations. In providing this report and performing the services in preparation of this report Azimuth accepts no responsibility in respect of the site described in this report or for any business decisions relating to the site, including decisions in respect of the management, operation, or any other aspect of the site. This report and the assessments and recommendations contained in it are intended for the sole and exclusive use of the Client. Any use of, reliance on, or decision made by a third party based on this report, or the services performed by Azimuth in preparation of this report is expressly prohibited, without prior written authorization from Azimuth. Without such prior written authorization, Azimuth accepts no liability or responsibility for any loss, damage, or liability of any kind that may be suffered or incurred by any third party as a result of that third party’s use of, reliance on, or any decision made based on this report or the services performed by Azimuth in preparation of this report. In preparing this report, Azimuth has assumed that the data or other information provided by others is factual and accurate. If any of the information is inaccurate, site conditions change, new information is discovered, and/or unexpected conditions are encountered in future work, then modifications by Azimuth to the findings, conclusions and recommendations of this report may be necessary. This report is time-sensitive and pertains to a specific site and a specific scope of work. It is not applicable to any other site, development or remediation other than that to which it specifically refers. Any change in the site, remediation or proposed development may necessitate a supplementary investigation and assessment. This report is subject to copyright. Reproduction or publication of this report, in whole or in part, without Azimuth’s prior written authorization, is not permitted.

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EXECUTIVE SUMMARY

First Nations communities and other stakeholders have expressed concern over mercury concentrations in fish from the Williston Reservoir watershed. Although the reservoir has had a provincial ‘fish consumption advisory’ in place for more than 20 years, no recent data have been collected to improve our understanding of mercury in fish of different sizes and locations. In spring 2015, Azimuth Consulting Group Partnership was retained by the Fish & Wildlife Compensation Program’s Peace Region (FWCP-Peace) to engage and consult with First Nations and other stakeholders to improve the available scientific information on fish mercury concentrations. The first step was a reconnaissance fish sampling program to collect fish for meristic (length and weight), metals (mercury and selenium) and stable isotope (nitrogen and carbon) analysis from specific species and areas within Williston Reservoir and its tributaries. This report describes results of the 2015 study on mercury and stable isotopes in bull trout (Salvelinus confluentus) from Ingenika River, Davis River and Scott Creek (reservoir), rainbow trout (Oncorhynchus. mykiss) from Thutade Lake (reference) and archived (2006) kokanee (O. nerka) from Finlay River, Pelly Creek and Germansen River (reservoir access) and Arctic Lake (a reference area). Bull trout – Twenty six bull trout were analysed from Scott Creek (6 fish) and ten fish each from Davis and Ingenika River. Mercury concentrations ranged from 0.08 to 0.91 mg/kg ww. Sample size of fish was small, so patterns in mercury concentration versus fish size, could not be made. Geographic differences may be apparent, with mean mercury concentration of Scott Creek fish (0.52 mg/kg) being higher than for Ingenika River (0.30 mg/kg) despite a smaller mean size (591 mm vs; 731 mm respectively). Davis River bull trout had a lower mercury concentration (mean of 0.22 mg/kg; 568 mm), about half that of Scott Creek. In all three populations, selenium concentration exceeded that of mercury, on a molar basis. Stable isotope ratios confirm that bull trout are top level predators of this system. Juveniles shift their diet from benthic invertebrates to kokanee as they get larger. Kokanee - Mercury concentration of Finlay River fish (n=25) ranged from 0.07 – 0.13 mg/kg ww with a mean of 0.09 mg/kg and no apparent correlation between mercury and fish size. Mercury in Pelly Creek and Germansen River kokanee (n=13) fell within a narrow range (0.05 – 0.06 mg/kg), similar to reference area Arctic Lake kokanee (0.05 mg/kg; n=5). Average size of kokanee from Arctic Lake (220 mm) was smaller than fish with access to Williston Reservoir (246 – 265 mm). Selenium concentrations in tissue were relatively much higher than for mercury. Stable isotope data showed that kokanee are intermediate in the food web, with a shift to higher trophic level invertebrates as fish get larger. Rainbow trout – Mercury concentration of Thutade Lake (isolated upper Finlay River reference area) rainbow trout (n=10) ranged from 0.03 – 0.09 mg/kg, with a mean of 0.05

vii June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program mg/kg and a slight positive correlation between fish size and mercury concentration. Selenium concentrations were much higher than for mercury with an abundance of selenium on a molar basis. Stable isotope data confirm that rainbow trout are intermediate in the food web relative to bull trout and similar to kokanee from Williston Reservoir, with a diet consisting of benthic and / or terrestrial invertebrates. Results of this study should be considered preliminary, as the intention is to combine information gathered from 2015 with new information collected from a more comprehensive study that will follow this work.

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1. INTRODUCTION

1.1. Background First Nations communities and other stakeholders have expressed concern over mercury concentrations in fish in Williston Reservoir. To address this concern, the Fish & Wildlife Compensation Program’s (FWCP) Peace Region carried out a strategic planning process in 2014. This exercise culminated in the development of a Basin Plan and six Action Plans, one of which was dedicated to mercury. The investigation of mercury in fish tissues in the Williston and Dinosaur Reservoir basins was given the highest priority of all the directed projects identified in the Action Plans. This report is the second investigation, carried out at a reconnaissance level, by the FWCP since 2014 to improve understanding of mercury in fish tissues in the Williston-Dinosaur basins. The existing provincial ‘fish consumption advisory’ was placed on Williston Reservoir at least 20 years ago and has not since been updated. The most recent dedicated survey of mercury analysis in fish on Williston Reservoir was in 2000 (Baker et al. 2002), so there is a desire to update the mercury data base and possibly re-visit the advisory. To initiate this process, Azimuth Consulting Group Partnership (Azimuth) was retained by the FWCP’s Peace Region to engage and consult with First Nations and other stakeholders (e.g., BC Hydro, provincial agencies, local outfitters, public stakeholders) regarding mercury concentrations in fish and other media in the Peace River watershed. Based on feedback from these groups, Azimuth produced a report which identified a series of ‘next steps’ to fulfill the project’s goals (Azimuth 2015). The goals are to improve the available scientific information on fish mercury concentrations within Williston Reservoir and possibly, Dinosaur Reservoir, communicate findings of the study, and support the provincial agencies responsible for revising the existing fish consumption advisory on Williston Reservoir. One of the ‘next steps’ was to conduct a reconnaissance fish sampling program in 2015. This involved opportunistic fish collections for meristic (length and weight), metals (mercury and selenium) and stable isotope (nitrogen and carbon) analysis. Information gained from the reconnaissance program would assist in designing a 2016 fish sampling program that targets specific species and areas within Williston Reservoir and relevant portions of the Peace River watershed.

1.2. Report Objectives

The goal of this phase of work is to provide preliminary information on mercury concentrations in fish in Williston Reservoir with low effort and cost. Findings will be used by the FWCP’s Peace Region to assist in designing a targeted fish study scheduled for 2016.

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Azimuth was retained by FWCP to coordinate fish tissue sample collection from: 1) select locations in the Williston Reservoir watershed on an opportunistic basis during a limited reconnaissance survey in 2015; and 2) process kokanee (Oncorhynchus nerka) captured from the reservoir in 2006 and archived, for laboratory assessment of total mercury, selenium and stable (carbon and nitrogen) isotopes. This document reports on the following:  The methodology used to collect tissue samples from fish using non-destructive (biopsy) and destructive (fillet) techniques and provision of ‘fish kits’ to certain groups;  Information around the benefits of including selenium and stable isotope analyses to accompany mercury data  Results of the lab analyses in tables and appropriate figures illustrating the relationship between mercury concentrations in fish and fish size  Results of trophic status of fish based on stable carbon and nitrogen isotopes  Cursory exploration of spatial trends (using graphical methods) for species collected from different areas (e.g., kokanee) –with a view to assist in planning the 2016 study  Determine selenium concentrations in fish to determine how concentrations compare to mercury, to inform data requirements for 2016 study.

2. METHODS

2.1. Overview

Reconnaissance fishing in Williston Reservoir tributaries occurred in August and September of 2015 and relied on opportunistically sampling via FWCP and other agencies’ programs already underway. “Piggy-backing” onto other programs provided a cost-effective means of collecting fish tissue samples. Groups willing to participate in the reconnaissance program were sent a “fish kit” which provided the tools and instructions (see Section 2.2) for field sampling fish tissue for laboratory metals and isotope analyses. Fish tissue samples that were collected for this program targeted rainbow trout (Oncorhynchus mykiss) and bull trout (Salvelinus confluentus).

Williston Reservoir fish tissue samples were also obtained from archived kokanee (O. nerka) captured in 2006 by staff of the FWCP’s Peace Region as part of kokanee assessment studies. These fish were made available to Azimuth in 2015 having been held frozen whole-body since capture. Individual fish were selected at random from the freezer facility at Forest, Lands, and Natural Resources Office’s (FLNRO) Prince George office, shipped on-ice to Azimuth’s office, where fish were defrosted, and then processed as per the standard operating procedures (see Section 2.2).

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2.2. Standard Operating Procedures Field methods for collecting tissues including tissue sampling, handling, and shipping are described in the standard operating procedure (SOP), Appendix A. This SOP was included in the fish kits provided by Azimuth to sampling groups for the reconnaissance program. The SOP was followed for 2015 and 2006 caught fish. Deviations from the SOP are discussed below in Sections 2.3. Briefly, upon capture fish were identified to species, and measured for weight (g; where possible) and length (mm) in the field. For 2015 captured fish, muscle tissue samples were collected in the field at time of fish capture, either non-lethally (biopsy punch; Baker et al. 2004) or lethally (fillet). For 2006 captured fish, muscle tissue samples were collected from defrosted whole-body fish in 2015 as fillets. Two samples were collected per fish: one for metals and one for stable isotopes analyses. Muscle tissue harvested from each individual fish was distributed to specific laboratories for analysis of mercury and selenium concentration (ALS Environmental, Burnaby, BC) and for stable carbon and nitrogen isotopes (SINLAB, Fredericton, NB). Both laboratories are nationally accredited and certified laboratories with a long history and expertise in conducting these kinds of analyses.

2.3. Deviations No body weight measurements were recorded for rainbow trout caught in the field. Approximately half of bull trout data were not weighed. Ageing structures were collected for most 2015 caught fish, but these data were not available to us at the time of writing. All kokanee included in this program were caught and frozen whole in 2006. Forty-three kokanee were selected for analysis in 2015. Original weight and length measurements were not available for all 2006 caught kokanee, so we re-measured weight and length during 2015 processing of kokanee tissue samples at the offices of Azimuth and only these data are reported here.

2.4. Laboratory Assessed Parameters

2.4.1. Mercury and Selenium Two muscle samples were collected per fish: one for metals (mercury and selenium) analysis and one for stable isotope (nitrogen and carbon) analysis. The scientific rationale for assessing selenium and stable isotopes as part of a mercury investigation are explained below. While the primary element of concern in this study is mercury, other elements are also important. The main chemical form of mercury in fish is ‘methylmercury’, which normally comprises at least 90% of all or total mercury measured in fish muscle tissue (Bloom 1992). Methylmercury is complicated (and costly) to analyse for, therefore, fish

3 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program tissue is typically analysed for ‘total mercury’. It is then conservatively assumed that what is measured is all ‘methylmercury’, the potentially more harmful form of this element. In recent years however, several researchers have cautioned that the amount or concentration of selenium in fish tissue is important to consider in mercury research (see Raymond et al. 2004, Beery and Ralston 2008, Ralston et al. 2008, Choi et al. 2008 and many others). It has been experimentally demonstrated that an abundance of selenium, relative to mercury has been found to protect against or mitigate the potentially harmful effects of methylmercury. This is true for several test species and has been postulated to be true for humans as well. Although still heavily debated, the generally accepted principal is that when there is an excess of selenium (on a molar basis) in tissue relative to mercury, the risks posed by methylmercury in fish tissue are much reduced or eliminated. The molar ratio of selenium to mercury is determined by comparing the number of atoms of selenium relative to the number of atoms of mercury in a tissue sample. Given that the atomic weight of selenium is 78.6 and the atomic weight of mercury is 200.6, this means that for an equivalent concentration (e.g., 1.0 mg/kg) in a mass of tissue, there would be 2.5 times more selenium atoms present than mercury atoms. Thus, on a molar ratio basis, if the concentration of mercury is 2.5 greater than the concentration of selenium, there are an equivalent number of atoms of each and the molar ratio is 1.0. At increasingly higher selenium concentrations relative to mercury, the ratio of selenium to mercury atoms, and therefore the molar ratio, becomes further increased.

2.4.2. Stable Isotopes Food web structure has a very strong influence on the magnitude of accumulation of some environmental contaminants in fish populations. Because top predator, carnivorous fish are at the end of a relatively long chain of food organisms (e.g., bacteria, plankton, invertebrates, small fish, large fish) there is an opportunity for fish to consume and accumulate nutrients as well as undesirable contaminants, such as mercury. This can result in higher concentrations of contaminants in large, old, predatory fish relative to small, young fish. One way of determining the food web relationship and ‘trophic position’ of an organism is to measure the ratio of stable carbon and nitrogen isotopes in its muscle tissue (i.e., stable isotopes analysis; SIA). Nitrogen isotopes (dN15) have been used as a means of distinguishing between and quantifying the trophic positions of consumers in aquatic systems (e.g., Vander Zanden et al. 2001, Herwig et al. 2004). Increasing stable nitrogen content in fish tissue indicates an increasing position in the food chain. For example, the nitrogen ‘signature’ in a mature lake trout will be higher than a rainbow trout or whitefish feeding at a lower trophic level. Carbon isotopes (dC13) have been used to trace the flow of energy through food webs and are particularly valuable in identifying energy flow paths (e.g., benthic vs. pelagic food chains) or dietary preferences (e.g., plants,

4 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program invertebrates, fish) of different species (e.g., Hecky and Hesslein 1995, Herwig et al. 2004). Together, the concentrations of stable nitrogen (dN15) and carbon (dC13) isotopes and their ratio relative to each other can provide good insights into trophic structure, based on feeding preferences. This information sheds valuable light on observed patterns in contaminant concentrations through the food web (Cabana and Rasmussen 1994, Cabana et al. 1994, Kidd et al. 1999). This is particularly important in Williston Reservoir because of changes in fish community structure since reservoir creation. The SIA results presented herein are cursory and based on raw dN15 and dC13 results only; corrections for baseline dN15 and lipid-related bias to dC13 were not conducted.

2.5. Data Management

2.5.1. Fish Catch Locations, Grouping and Categorizing UTMs for sampling locations were usually recorded on data sheets provided by the collector, but not always. However, approximate locations were always well known and when locations weren’t precisely identified, best judgement was used to determine the most likely capture location and verified with the collector where possible. It was important to accurately identify a location in order to distinguish between areas where fish have access to Williston Reservoir versus possible ‘reference’ locations, where fish do not have access to the reservoir. Where catch locations were in close proximity, of the same sampling year, and without barriers to the reservoir1, catch locations were combined for simplification of data analysis (Table 2-1). For example, in 2006 kokanee were collected from seven separate catch locations. Five of these were in relatively close proximity on the Finlay River, so these were grouped together to form a single data set, independent from fish caught on the Ingenika River and Germansen River, much further south. Fish catch locations were categorized as either influenced by Williston Reservoir (no barriers preventing fish from entering the reservoir) or as reference (barriers prevent fish from entering the reservoir) (Table 2-1).

2.5.2. Data Manipulations Data manipulations and graphical outputs were conducted using R statistical software. Fish condition (k) was calculated as:

k = (10^5*body weight)/(fork length)^3

1 A large falls is located a few km downstream of Thutade Lake on the Finlay River. Any fish caught above the falls (Thutade Lake) are considered reference fish, and any caught below are considered to have unfettered access to Williston Reservoir.

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Mercury and selenium data were provided by the lab in units of dry weight for biopsy punch samples for bull trout, the only species sampled non-destructively. The conversion of dry weight to wet weight was achieved by employing the generic moisture content of salmonids (78.5%) as follows: wet weight = dry weight * (1 - 0.785)

2.6. Quality Assurance Quality Control The issuance of the SOP and associated data sheets as a component of the fish kit was the primary means for field QA measures. All samples were sent to the laboratories in one shipment from Azimuth’s office, to ensure correct and clear labeling of all samples and consistently filled chain-of-custody forms for each laboratory. All certified reference material and laboratory duplicates met the ALS’s data quality objectives for mercury and selenium data. All laboratory duplicates and standards met SINLAB’s data quality objectives for stable nitrogen and carbon isotope values.

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Table 2-1. Summary of fish catch locations and grouping for 2015 and 2006 data.

Catch Location (as recorded on field Consolidated Location (for data Williston Reservoir Access? Species Year datasheet) analysis and mapping) (Accessible/Reference) Caught Caught Thutade Lake Rainbow Thutade Lake - N of Attichika Cr. Thutade Lake Reference 2015 trout Thutade Lake - W of Attichika Cr. Ingenika River -1 Ingenika River -2 Ingenika River Influenced Bull trout 2015 Ingenika River -3 Davis River Davis River Influenced Bull trout 2015 Scott Creek Scott Creek Influenced Bull trout 2015 Arctic Lake Arctic Lake Reference Kokanee 2006 Bower Creek - 100m US of Finlay River Finlay River Finlay Slough Finlay River Influenced Kokanee 2006 Russel Creek - 100m US of Finlay River Tsaydiz Creek Germansen River Germansen River Influenced Kokanee 2006 Pelly Creek - 500m US of Ingenika camp Pelly Creek Influenced Kokanee 2006

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3. RESULTS & DISCUSSION

Fish capture locations from 2006 and 2015 are summarized in Table 2-1 and depicted on the map of Williston Reservoir and surrounding area in Figure 3-1. Biological results are summarized by species and location caught in Table 3-1. Raw data for individual fish are provided in Appendix B. Three species of fish were captured during the reconnaissance program. Field and laboratory results by species are discussed below.

3.1. Rainbow trout Ten rainbow trout were collected in Thutade Lake in 2015. Thutade Lake connects Williston Reservoir via Finlay River, upstream of an impassible falls that is only a few km downstream of the lake in the headwaters of the Finlay River. This falls acts as a barrier to fish movement, therefore all rainbow trout caught in Thutade Lake were considered as reference fish, with no access from Williston Reservoir. Note however, that this lake is near the closed Kemess copper-gold open pit mine; any influence from that mine on metals in fish is unknown, but not likely relevant for mercury. Rainbow trout field and laboratory measurements are summarized in Table 3-1 and Figures 3-2 through Figure 3-4. Tissue samples were collected using destructive means to obtain small fillets because of their small body size, ranging in length from 111 – 156 mm. No weight data were collected, however because the scale was not suitable for small fish. Trout of this length typically weigh less than 140 g. Condition factor could not be calculated because of the lack of weight data. Mercury concentration of Thutade Lake rainbow trout ranged from 0.03 – 0.09 mg/kg wet weight (ww) with a mean of 0.05 mg/kg (Table 3-1). Despite the small sample size, there appeared to be a slight positive correlation between size and mercury concentration (Figure 3-2). Selenium concentration ranged from 0.72 – 1.26 mg/kg ww, with a mean of 0.90 mg/kg. The relationship between total selenium concentration (mg/kg) and fish length (mm) were plotted in Figure 3-3 and showed that they were tightly grouped, with a possible positive correlation with increasing fish size. Selenium concentrations were approximately 10 – 25 times higher than mercury concentrations in the same fish. Thus, on a molar basis, the average selenium molar content was 47 times higher than molar content of mercury for rainbow trout from this lake, much higher than for other species in this study. Stable nitrogen isotope (d15N) concentration of rainbow trout ranged from 6.9 – 8.4 with a mean of 7.5 (Table 3-1), with a small positive correlation with increasing length (Figure 3-4). The magnitude of dN15 suggests that rainbow trout are intermediate in the food web relative to a top predator such as bull trout (dN15 = 11.9 from Williston; Table

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3-1) and more similar to a Williston Reservoir kokanee in terms of trophic position (but have different dietary preferences). The slight positive relationship between fish size and dN15 suggests that as rainbow trout get larger, they shift to prey of a slightly higher trophic level. The relationship between stable nitrogen and carbon isotopes (Figure 3-5) shows a conspicuous grouping for rainbow trout, suggesting that the Thutade Lake fish had fairly similar diets. The dC13 values for rainbow trout are more enriched than those seen for bull trout and kokanee, which is likely more consistent with a diet of benthic invertebrates (e.g., emergent adults) and/or terrestrial (which are generally more enriched) carbon sources; more comprehensive SIA work would need to be conducted to elucidate this further.

3.2. Bull trout Bull trout samples from three tributaries of Williston Reservoir in 2015: Scott Creek (six fish) in the Parsnip Reach, Davis River (10 fish) and Ingenika River (10 fish) within the Finlay Reach (Figure 3-1). Bull trout from these locations have no barriers to reservoir access. A total of 26 bull trout were assessed for metals and isotope content using non- destructive biopsy techniques. Bull trout field and laboratory measurements are summarized in Table 3-1 and Figures 3-6 through Figure 3-9. Bull trout body lengths ranged from 340 to 790 mm (Table 3-1), and body weights ranged from 300 to 4460 g, although not all bull trout were weighed. No weights were collected for Ingenika River bull trout and only three bull trout weights were recorded at Scott Creek. Based on the length-weight relationship of bull trout (Figure 3-6), one Scott Creek fish fell well outside of the pattern of the rest of the population, indicating that either a length or weight were recorded in error. Consequently, this fish was excluded from length and weight summary data metrics in Table 3-1, and highlighted (circled data point) in Figures 3-6 through 3-9 (i.e., as a possible outlier). Otherwise, bull trout weight to length relationships appeared reasonable as condition (k) was generally within acceptable range (> 0.8). Condition of Scott Creek bull trout (mean = 0.83) was lower than for Davis River (1.01), although sample size was much too small (n = 2) to be definitive. Mercury concentrations of individual bull trout ranged from 0.08 to 0.91 mg/kg ww. Sample size of fish was small, so it is difficult to say much about patterns in mercury concentration versus fish size. For example, mean mercury concentration of Scott Creek fish (0.52 mg/kg; 591 mm) was higher than for Ingenika River (0.30 mg/kg; 731 mm) despite much smaller fish size. Davis River (0.22 mg/kg; 568 mm) had the lowest mean mercury concentration, about half that of Scott Creek at a similar size (Table 3-1).

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Davis Bay was the only location in the Baker et al. (2002) investigation where bull trout were captured. While only two bull trout were captured, both fish had higher mercury concentrations than in the present study (0.48 mg/kg, 674 mm; 0.26 mg/kg, 360 mm). Amongst the largest bull trout (~700 – 800 mm) mercury concentrations varied widely (0.18 – 0.91) (Figure 3-7). This might be explained by either the age range for these fish, as old fish continue to accumulate mercury even though they may grow very slowly, or by environment, as Ingenika River fish appear to have comparatively lower mercury content. Mercury concentrations were substantially higher in bull trout than that of the other species in this program, with bull trout having, on average, mercury concentrations an order of magnitude greater than rainbow trout or kokanee. This is typical and explained by diet and stable isotope signatures. Selenium concentration ranged from 0.23 – 0.54 mg/kg and did not show any correlation with increasing fish size (Figure 3-8). These concentrations are similar to or slightly higher than mercury concentration for the same fish. Thus, on a molar basis, there is an excess of selenium relative to mercury atoms. The mean molar ratio of selenium to mercury ranged from 1.5 for Scott Creek, 3.3 for Ingenika and 5.0 for Davis River bull trout. Stable nitrogen isotope concentration of bull trout ranged from 10.2 – 12.7‰ (Table 3- 1), and are representative of the top predator in the system. There is no discernable relationship between d15N and length (Figure 3-9), with the exception of two small fish caught in Scott Creek that have notably lower d15N than the other fish. The lower d15N signature is characteristic of fish that feed lower on the food chain relative to the larger bull trout. This suggests that, at least in the Scott Creek tributary, small and large fish have different diets. Once they reach a certain size bull trout may shift to higher trophic prey organisms such as small fish. The relationship between stable nitrogen and carbon isotopes (Figure 3-5) shows two groups of bull trout: the main group and the two smallest fish from Scott Creek. Interestingly, the d13C results provide additional evidence of a dietary shift occurring in bull trout, with the diet of the two smaller Scott Creek fish characterized by more enriched d13C relative to the main group of larger bull trout. The main group appears to feed more exclusively on kokanee (i.e., the pelagic food chain), while the two smaller Scott Creek fish are likely feeding more on benthic invertebrates (i.e., the benthic food chain); more intensive SIA work would need to be conducted to better understand these potential trends.

3.3. Kokanee In 2006, kokanee were collected from three Williston Reservoir tributaries and one reference location (Figure 3-1). Finlay River and Pelly Creek are tributaries of the Finlay Reach of Williston Reservoir, while Germansen River is a tributary that meets the reservoir near the intersection of all three reservoir reaches. The reference location,

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Arctic Lake, is located south east of the Parsnip Reach of Williston Reservoir. Forty- three (43) frozen kokanee caught in 2006 were provided to Azimuth for processing; meristic parameters and mercury data are summarized in Table 3-1 and Figures 3-10 through 3-12. Kokanee from Arctic Lake were smaller than kokanee from the three reservoir locations (Figure 3-10). Overall the length to weight relationship was consistent for all kokanee regardless of location caught (Figure 3-11). Fish condition ranged widely from 0.8 – 1.5. This is likely attributable to kokanee morphology. Spawning males have a pronounced hump and deep body relative to length, while females do not (see photos in Appendix C). Additionally, reference area fish were caught in June and were likely not mature at time of field sampling (Appendix C). Mercury concentration of reference area kokanee ranged within a narrow range, from 0.05 – 0.06 mg/kg ww with a mean of 0.05 mg/kg. Average size (220 mm) was smaller than fish with access to Williston Reservoir (246 – 265 mm). Mercury concentrations of individual fish there ranged from 0.04 – 0.13 mg/kg ww. Mean mercury concentration of Finlay River fish was 0.09 mg/kg (Table 3-1). There did not appear to be any correlation between size and mercury concentration, although Finlay River fish may have a higher body burden than others (Figure 3-12). Kokanee selenium concentrations ranged from 0.08 – 0.51 mg/kg ww (Table 3-1), generally much higher than mercury concentration from the same fish. Reference fish from Arctic Lake had lower selenium concentrations relative to kokanee from other areas (Figure 3-13). Selenium to mercury ratios were therefore much higher in kokanee from Williston Reservoir than reference fish. On a molar ratio basis, the mean selenium to mercury ratio was higher for Finlay River (11x), Germansen River (15x) and Pelly River (16x) than for Arctic Lake (5x), although all fish had an abundance of selenium in muscle tissue relative to mercury. Stable nitrogen isotope of kokanee ranged from 6.8 – 10‰ (i.e., parts per thousand). Reference area kokanee were at the lower end of this range and had similar d15N values to rainbow trout. There was a clear positive correlation with increasing length (Figure 3- 14). The magnitude of dN15 suggests that kokanee are intermediate in the food web relative to a top predator such as bull trout. The positive relationship between fish size and dN15 suggests that as kokanee get larger, they may shift to higher food web organisms (e.g., larger, predatory zooplankton). The relationship between stable nitrogen and carbon isotopes (Figure 3-5) shows two groups of kokanee: the main group (consisting of fish from Germansen River, Pelly Creek and Finlay River) and the reference group from Arctic Lake. While the dN15 results suggest that Arctic Lake fish are feeding lower in the food chain, it is also possible that dN15 values are naturally lower in that system; SIA results can be corrected for differences in baseline d15N values (i.e., by incorporating SIA data from benthos and zooplankton) to remove this natural bias where it occurs. From a dC13 perspective, all

4 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program kokanee showed more depleted diets, which is usually consistent with the pelagic food chain. As discussed in Section 3.2, the bull trout results showed fairly similar dC13 results, which highlights the well-established predator-prey relationship between bull trout and kokanee.

5 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Table 3-1. Summary of length (mm), weight (g), condition factor, mercury (mg/kg ww), selenium (mg/kg ww) and stable nitrogen and carbon isotopes for rainbow trout and bull trout (2015) and kokanee (2006).

Length (mm) Weight (g) Condition* Species Location sample size average minimum maximum S.D. sample size average minimum maximum S.D. sample size average minimum maximum S.D. Ingenika River 10 731 665 785 40 0 - - - - 0 - - - - Bull Trout Davis River 10 568 440 755 110 10 1968 1050 4350 1108 10 1.01 0.80 1.23 0.12 Scott Creek** 5 591 340 790 188 2 2380 300 4460 2942 2 0.83 0.76 0.90 0.10 Rainbow Thutade Lake 10 129 111 156 14 0 - - - - 0 - - - - Trout Arctic Lake 5 220 210 225 6 5 106 95 112 8 5 1.00 0.98 1.04 0.03 Germansen River 7 265 234 301 21 7 221 173 317 47 7 1.18 1.09 1.51 0.15 Kokanee Pelly Creek 6 254 232 266 12 6 207 173 276 40 6 1.26 1.06 1.47 0.17 Finlay River 25 246 220 290 16 25 177 106 303 43 25 1.18 0.81 1.39 0.14 Hg (ww) Se (ww) sample size average minimum maximum S.D. sample size average minimum maximum S.D. Ingenika River 10 0.30 0.18 0.47 0.09 10 0.39 0.31 0.54 0.07 Bull Trout Davis River 10 0.22 0.08 0.58 0.18 10 0.43 0.38 0.52 0.05 Scott Creek 6 0.52 0.16 0.91 0.31 6 0.31 0.23 0.42 0.06 Rainbow Thutade Lake 10 0.05 0.03 0.09 0.02 10 0.90 0.72 1.26 0.17 Trout Arctic Lake 5 0.05 0.05 0.06 0.00 5 0.10 0.08 0.13 0.02 Germansen River 7 0.06 0.05 0.08 0.01 7 0.38 0.29 0.44 0.05 Kokanee Pelly Creek 6 0.06 0.04 0.08 0.01 6 0.41 0.33 0.51 0.07 Finlay River 25 0.09 0.07 0.13 0.02 25 0.40 0.25 0.50 0.08 d13C.m d15N.m sample size average minimum maximum S.D. sample size average minimum maximum S.D. Ingenika River 10 -31.1 -32.0 -29.9 0.7 10 11.9 11.6 12.4 0.27 Bull Trout Davis River 10 -31.2 -32.0 -30.5 0.5 10 11.9 11.4 12.7 0.46 Scott Creek 6 -29.7 -30.7 -27.9 1.1 6 11.5 10.2 12.3 0.89 Rainbow Thutade Lake 10 -24.7 -26.2 -23.5 0.8 10 7.5 6.9 8.4 0.54 Trout Arctic Lake 5 -32.0 -32.8 -31.4 0.6 5 7.4 6.8 7.9 0.53 Germansen River 7 -32.3 -33.2 -31.3 0.5 7 9.3 8.4 10.3 0.69 Kokanee Pelly Creek 6 -32.0 -32.5 -31.2 0.5 6 9.1 8.7 9.9 0.50 Finlay River 25 -31.5 -32.0 -30.9 0.3 25 8.9 8.3 9.9 0.42

* Condition calculated as (10^4)*(weight)/(length^3) ** One fish was identified as an outlier (K<0.7). Length and weight information for this fish was not included in length, weight and condition metrics.

6 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-1. Overview of fish capture locations.

7 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-2. Total mercury concentration (mg/kg ww) of tissue versus fork length (mm) for individual rainbow trout caught in Thutade Lake.

0.100

0.075

0.050

0.025

Total Mercury (mg/kg wet weight) wet (mg/kg Mercury Total

0.000

50 100 150 200 Fork Length (mm)

Figure 3-3. Total selenium concentration (mg/kg ww) of tissue versus fork length (mm) for individual rainbow trout caught in Thutade Lake.

1.25

1.00

0.75

Total Selenium (mg/kg wet weight) wet (mg/kg Selenium Total

0.50

50 100 150 200 Fork Length (mm)

8 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-4. Relationship between δ15N and fish length (mm) for individual rainbow trout caught in Thutade Lake.

9

8

d15N (0/00) 7

6

50 100 150 200 Fork Length (mm)

9 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-5. Relationship between δ15N and δ13C for individual rainbow trout (Thutade Lake), kokanee (2006) and bull trout, Williston Reservoir.

Species BULL RNBW KOKA

Arctic Lake Finlay River Germansen River Scott Creek Location Davis River Ingenika River Pelly Creek Thutade Lake

12

10

d15N(0/00)

8

6

-35.0 -32.5 -30.0 -27.5 -25.0 -22.5 d13C (0/00)

Circled data point = Condition outlier (K < 0.7).

10 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-6. Weight (g) versus length (mm) for individual bull trout caught in tributaries of Williston Reservoir.

Location Davis River Scott Creek Ingenika River 5000

4000

3000

Weight (g) 2000

1000

0

300 400 500 600 700 800 Fork Length (mm)

Figure 3-7. Relationship between total mercury concentration (mg/kg ww) and fork length (mm) for individual bull trout caught in Williston Reservoir tributaries.

Location Davis River Scott Creek Ingenika River 1.00

0.75

0.50

0.25

Total Mercury (mg/kg wet weight) wet (mg/kg Mercury Total

0.00

300 400 500 600 700 800 Fork Length (mm) Circled data point = Condition outlier (K < 0.7).

11 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-8. Total selenium concentration (mg/kg ww) versus fish length mm) for individual bull trout caught in tributaries of Williston Reservoir.

Location Davis River Scott Creek Ingenika River

0.6

0.4

0.2

Total Selenium (mg/kg wet weight) wet (mg/kg Selenium Total

0.0

300 400 500 600 700 800 Fork Length (mm)

Figure 3-9. Relationship between δ15N and fish length (mm) for individual bull trout caught in tributaries of Williston Reservoir.

Location Davis River Scott Creek Ingenika River

13

12

d15N (0/00)

11

10

300 400 500 600 700 800 Fork Length (mm)

Circled data point = Condition outlier (K < 0.7)

12 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-10. Distribution of 2006 fish length data for kokanee among areas.

300

250

Fork Length (mm) Length Fork

200 n = 5 n = 7 n = 6 n = 25

Arctic Lake Germansen River Pelly Creek Finlay River Location

Figure 3-11. Weight versus length for individual kokanee caught in tributaries of Williston Reservoir.

Location Arctic Lake Germansen River Pelly Creek Finlay River 350

300

250

200

Weight (g)

150

100

50

200 240 280 320 Fork Length (mm)

13 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-12. Relationship between total mercury concentration (mg/kg ww) and fork length for individual kokanee in tributaries of Williston Reservoir, 2006. Location Arctic Lake Germansen River Pelly Creek Finlay River 0.15

0.10

0.05

Total Mercury (mg/kg wet weight) wet (mg/kg Mercury Total

0.00

200 240 280 320 Fork Length (mm)

Figure 3-13. Relationship between total selenium concentration (mg/kg ww) and fork length for individual kokanee in tributaries of Williston Reservoir, 2006. Location Arctic Lake Germansen River Pelly Creek Finlay River

0.6

0.4

0.2

Total Selenium (mg/kg wet weight) wet (mg/kg Selenium Total

0.0

200 240 280 320 Fork Length (mm)

14 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Figure 3-14. Relationship between δ15N and fish length (mm) for individual kokanee caught in tributaries of Williston Reservoir, 2006.

Fishloc Arctic Lake Germansen River Pelly Creek Finlay River 11

10

9

8

d15N (0/00)

7

6

200 240 280 320 Fork Length (mm)

15 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

4. REFERENCES

Azimuth Consulting Group (Azimuth) 2015. Williston Reservoir Watershed – Fish Mercury Consultation and Next Steps. A document prepared by Azimuth Consulting Group, Vancouver BC for BC Hydro, Vancouver, BC. March 2015. Baker, R.F., R.R. Turner and D. Gass. 2002. Mercury in Environmental Media of Finlay Reach, Williston Reservoir, 2000-2001 Data Summary. A report prepared by EVS Environment Consultants North Vancouver for BC Hydro, Burnaby, March 2002. Baker, R.F., P.A. Blanchfield, M.J. Paterson, R.J. Fudge and L. Wesson. 2004. Evaluation of non-lethal methods for the analysis of mercury in fish tissue. Trans. Am. Fish. Soc. 133: 568 – 576.

Berry, M.J. and N.V. Ralston. 2008. Mercury toxicity and the mitigating role of selenium. EcoHealth 5: 456 – 459.

Bloom, N. 1992. On the chemical form of mercury in edible fish and marine invertebrate tissue. Can. J. Fish. Aquat. Sci: 49: 1010-1017. Cabana, G. and J.B. Rasmussen. 1994. Modeling food chain structure and contaminant bioaccumulation using stable nitrogen isotopes. Nature 372: 255-257. Cabana, G., A. Tremblay, J. Kalff, and J.B. Rasmussen. 1994. Pelagic food chain structure in Ontario Lakes: A determinant of mercury levels in lake trout (Salvelinus namaycush). Can. J. Fish. Aquat. Sci. 51: 381-389.

Choi, A.L, E. Budtz-Jorgensen, P.J. Jorgensen, U. Steuerwald, F. Debes, P. Weibe and P. Grandjean. 2008. Selenium as a potential protective factor against mercury developmental neurotoxicity. Enviro. Res. 107: 45 – 52. Hecky, R.E. and R.H. Hesslein. 1995. Contributions of benthic algae to lake food webs as revealed by stable isotope analysis. Journal of the North American Benthological Society 14: 631-653. Herwig, B.R., D.A. Soluk, J.M. Dettmers and D.H. Wahl. 2004. Trophic structure and energy flow in backwater lakes of two large floodplain rivers assessed using stable isotopes. Can. J. Fish. Aquat. Sci. 61: 12-22. Kidd, K.A., M.J. Paterson, R.H. Hesslein, D.C.G. Muir and R.E. Hecky. 1999. Effects of northern pike (Esox lucius) additions on pollutant accumulation and food web structure, as determined by d13C and d15N, in a eutrophic and an oligotrophic lake. Can. J. Fish. Aquat. Sci. 56: 2193-2202. Ralston, N.V., C.R. Ralston, J.L. Blackwell III and L.J. Raymond. 2008. Dietary and tissue selenium in relation to methylmercury toxicity. NeuroToxicology 29: 802 – 811.

16 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

Raymond, L.J. and N.V. Ralston. 2004. Mercury: selenium interactions and health implications. SMDJ Seychelles Medical and Dental Journal, Sec. Issue, Vol. 7 (1), November, 2004.

Vander Zanden, M.J. and J.B. Rasmussen. 2001. Variations in d15N and d13C trophic fractionation: Implications for aquatic food web studies. Limnology and Oceanography 46: 2061-2066.

17 June 2016 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

APPENDIX A – FISH TISSUE COLLECTION & RECORDING PROCEDURES

18 June 2016 FISH TISSUE COLLECTION & RECORDING PROCEDURES

Version: 14 August 2015

Sampling Kits Each sampling kit is contained within a blue Rubbermaid tote and has the following materials:

 Spring scale (some kits)  Measuring board (some kits; outside the tote)  Measuring tape  Disposable nitrile gloves  Anesthetic – clove oil & rubbing alcohol, with a small graduated measuring tube  Scalpel and disposable scalpel blades  Fillet knife  Biopsy punches  Plastic cutting board  Forceps  Small vials for biopsy samples  Waterproof sticky labels for small vials  Whirl‐Pak© bags for fillet samples  Bottle of liquid bandage  Soap and scrub brush  Clipboard with these procedures & datasheets  Sharpie markers and lead pencils  Garbage container for sharps; garbage bag  Extra Ziploc bags

Other optional gear includes:  2 large tubs (one for anesthetizing; one for recovery)  2 battery‐powered oxygen stones

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Record Keeping If you are conducting a creel survey, use the datasheet labelled “Creel Survey Records”. The datasheets are printed on waterproof paper; a pencil should be used to write on this type of paper. Fill in the following information:

 Recorder Information: o Date the record was taken o Name of the person recording the data  Catch Information: o Date the fish was caught o Name of the person who caught the fish o Description of the approximate location where the fish was caught (include location GPS coordinates if known). Include which reach of Williston Reservoir if appropriate (i.e., Finlay, Parsnip, Peace) o Fish species that was caught (use 4‐letter abbreviations listed on the datasheet); list all species caught by each fisher on a separate line o The number of fish caught for each species  Consumption Information: o Fish species that is eaten (use 4‐letter abbreviations listed on the datasheet) o The number of meals per week for each fish species consumed (“frequency”) o The size of each meal (in grams if possible)

If you are sampling fish tissue, use the datasheet labelled “Fish Tissue Sample Records”. The datasheets are printed on waterproof paper; a pencil should be used to write on this type of paper. Fill in a separate line for every individual fish sampled. Fill in the following information:

 Recorder Information: o Date the record was taken o Name of the person recording the data  Fishing Information: o Date the fish was caught o Name of the person who caught the fish o Description of the approximate location where the fish was caught (include location GPS coordinates if known). Include which reach of Williston Reservoir if appropriate (i.e., Finlay, Parsnip, Peace)  Fish Sample Information: o Fish species sampled (use 4‐letter abbreviations listed on the datasheet) o Full length of the fish in millimeters (mm) o Weight of the fish in grams (g)

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o Indicate whether a biopsy (B) or a fillet (F) sample was taken o Sample ID that is written on the sample (vial or bag); assign an ID using the 4‐ letter fish species code, followed by the recorder’s 2‐letter initials, followed by a sequential number, then either B (if biopsy) or F (if fillet) (e.g., the first lake trout recorded by Maggie McConnell that was sampled by biopsy would be: LKTR‐ MM‐01‐B)

Biopsy or Fillet Sample? When sampling fish tissue, decide whether a biopsy sample or a fillet sample will be collected. If fish are already dead or will be sacrificed, then it is preferable to collect a fillet sample. If fish are being caught‐and‐released alive or are caught for consumption and the fisher would prefer that only a small sample be taken from the fish, then it is preferable to collect a biopsy sample.

Biopsy Sampling Procedures This procedure is typically conducted on live fish that are anesthetized then released back into the water after recovery. This procedure is preferably done with two people, one person to handle the fish and one person to record the data. This procedure can also be conducted on dead fish if a smaller sample is preferred – in this case, skip steps 2, 3, 7 & 8. 1. Put on a clean pair of nitrile gloves and ensure that all equipment is clean (and new [sterile] for the biopsy punch and scalpel). 2. Prepare the fish anesthetic bath in a large tub (or the Rubbermaid tote can be emptied out and used for this). To do this, collect about 10 liters (L) of lake water into the tub (or this is equivalent to filling the Rubbermaid tote about ¼ full). Then mix 0.4 milliliters (mL) of clove oil with 4 milliliters (mL) of rubbing alcohol (use the small graduated measuring tube provided to measure and mix these together). Add the clove oil/rubbing alcohol mixture to the lake water. If the bath seems to shallow, then repeat the above to double the quantity of water and anesthetic. The anesthetic bath should be replaced each day if sampling over a number of days; in hot weather the bath may need more frequent changing. Battery‐operated oxygen stones can be used to increase oxygenation in the anesthetic bath. 3. Capture a live fish and place in the anesthetic bath for 1 – 2 minutes. 4. Measure and record its total length (mm) and total weight (g). If using a spring scale, place the fish in a large Ziploc bag to hang from the scale. Subtract the weight of the bag, or use the “tare” function before adding the fish.

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5. Place the fish on its right side. Using a scalpel with a new blade, gently scrape away several scales from the left side of the fish, just beneath the dorsal fin (approximately in the area shown as X X X in the fish diagram below).

6. Using a clean biopsy punch, extract three individual tissue “plugs” from the area where the scales were scraped away, removing each tissue plug from the biopsy punch and placing them on a clean plastic cutting board for processing. 7. Before processing the samples, seal up the 3 punch holes in the fish by placing a few drops of the liquid bandage ointment into each hole (or whatever amount is required to seal the wound). Wait a minute or two for the bandage to dry. 8. Return the fish to water but hold it in the lake water until it has recovered from the anesthetic. Gently move the fish through the water to allow water to flow across the gills. Note that a second tub, filled with well‐oxygenated water, can be helpful as a recovery bath to hold fish after sampling, before returning it to the lake. Battery‐ operated oxygen stones can be used to increase oxygenation in the recovery tub. 9. Using the same scalpel as above, cut away the outer skin from the 3 tissue plugs. Use the forceps to transfer two tissue plugs into one small sampling vial and transfer the third tissue plug into a second vial. 10. Seal the vials and label them as indicated in the record keeping section above, using the waterproof sticky labels and the Sharpie marker provided. Both vials are labelled with

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the same ID; however, indicate on the label which vial has one (1) plug and which vial has (2) plugs. 11. Put the tissue sample vials on ice in a cooler in the short term and transfer to a freezer as soon as possible. It is preferable to organize the vials into Ziploc bags by species/date etc. to minimize the chances of vials getting lost.

12. Clean the cutting board and the forceps for the next sample. To do this, use a drop of the soap (it’s quite concentrated) and the brush to scrub clean. Use the lake water for rinsing (this soap is safe for the environment).

13. Discard the scalpel blade (not the handle), the biopsy punch, into the container marked “Garbage” and the disposable gloves into the bag marked “Garbage”. New ones are used for the next fish.

Fillet Sampling Procedures This procedure is only conducted on dead fish that are being sacrificed for science or for consumption. This procedure can be done with one person as there is no time pressure to work fast since the fish is already dead. 1. Put on a clean pair of nitrile gloves and ensure that all equipment is clean (and new [sterile] for the scalpel). 2. Measure and record the fish’s total length (mm) and total weight (g). If using a spring scale, place the fish in a large Ziploc bag to hang from the scale. Subtract the weight of the bag, or use the “tare” function before adding the fish. 3. Place the fish on its right side. Using the fillet knife, cut out a small section of muscle (aim for 10 – 15 grams) from the area just beneath the dorsal fin on the left side of the fish (same area as shown in the above diagram) and place it onto a clean plastic cutting board for processing. 4. Using a scalpel with a new blade, cut away the outer skin from the muscle. Cut the piece of muscle in two. Use the forceps to transfer each piece into a Whirl‐Pak© sample bag. 5. Seal the bags and label them as indicated in the record keeping section above, using a sharpie marker (write directly on the Whirl‐Pak© bag in the white section). Both bags are labelled with the same ID. 6. Put the tissue sample bags on ice in a cooler in the short term and transfer to a freezer when possible.

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7. Clean the fillet knife, cutting board, and the forceps for the next sample. To do this, use a drop of the soap (it’s quite concentrated) and the brush to scrub clean. Use the lake water for rinsing (this soap is safe for the environment).

8. Discard the scalpel blade (not the handle) into the container marked “Garbage” and the disposable gloves into the bag marked “Garbage”. New ones are used for the next fish.

Storage and Shipping

 All samples should be frozen as soon as possible after sampling

 Contact Maggie McConnell or Gary Mann at Azimuth Consulting Group in Vancouver when your sampling program is finished (if short term sampling) or at the end of each month (if ongoing sampling) to coordinate a shipping plan:

o Office phone: 604‐730‐1220

o Email: [email protected] or [email protected]

 We will send you shipping instructions at that time; but you will likely be shipping samples to Azimuth’s office

 Samples need to be kept frozen while shipping – use a cooler and ice packs (lots) and select a one‐day shipping service if possible

 Please include all the data sheets that are associated with the samples in the cooler

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Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

APPENDIX B – RAW INDIVIDUAL FISH DATA AND LABORATORY REPORTS (ALS AND SINLAB)

19 June 2016 Appendix B. Raw field and laboratory data for fish caught in 2015 and 2006, Williston Reservoir Mercury Reconnaissance Program.

Length Weight Maturity Year Sample ID Catch Location Catch Date Species1 (mm) (g) Condition Comments d13C d15N moist T.Hg.dw 2 T.Hg.ww T.Se.dw 2 T.Se.ww 2006 ARC-49-06 Arctic Lake 21-Jun-06 KOKA 210 95 1.03 -32.84 7.47 75 0.75 0.046 0.089 2006 ARC-05-06 Arctic Lake 21-Jun-06 KOKA 218 102 0.98 -32.42 7.92 76.7 0.767 0.047 0.083 2006 ARC-08-06 Arctic Lake 21-Jun-06 KOKA 220 111 1.04 -32.05 6.86 77.3 0.773 0.046 0.085 2006 ARC-07-06 Arctic Lake 21-Jun-06 KOKA 225 112 0.98 -31.52 7.85 73.5 0.735 0.054 0.134 2006 ARC-33-06 Arctic Lake 21-Jun-06 KOKA 225 112 0.98 -31.41 6.79 74.7 0.747 0.055 0.100 2006 BOW-31-06 Bower Creek - 100m US of Finlay River 7-Sep-06 KOKA 230 150 1.23 Mature; eggs -31.17 8.52 75.5 0.755 0.097 0.490 2006 BOW-26-06 Bower Creek - 100m US of Finlay River 7-Sep-06 KOKA 240 170 1.23 Mature -31.38 8.90 77.4 0.774 0.087 0.476 2006 BOW-22-06 Bower Creek - 100m US of Finlay River 7-Sep-06 KOKA 255 201 1.21 -31.69 9.06 80.7 0.807 0.075 0.367 2006 BOW-11-06 Bower Creek - 100m US of Finlay River 7-Sep-06 KOKA 261 247 1.39 Spent -31.40 9.43 79.8 0.798 0.078 0.450 2006 BOW-05-06 Bower Creek - 100m US of Finlay River 7-Sep-06 KOKA 278 229 1.07 Full of eggs -31.95 9.95 78.7 0.787 0.085 0.432 2006 FIN-23-06 Finlay River 26-Oct-06 KOKA 220 106 0.99 -30.88 8.63 86 0.86 0.134 0.341 2006 FIN-48-06 Finlay River 26-Oct-06 KOKA 230 131 1.08 -31.15 8.85 85.7 0.857 0.092 0.278 2006 FIN-50-06 Finlay River 26-Oct-06 KOKA 230 132 1.08 -31.19 8.34 85.6 0.856 0.113 0.294 2006 FIN-44-06 Finlay River 26-Oct-06 KOKA 245 158 1.08 -31.18 8.42 82.7 0.827 0.106 0.365 2006 FSL-05-06 Finlay Slough 3-Oct-06 KOKA 235 136 1.05 -31.23 8.76 86.7 0.867 0.085 0.269 2006 FSL-08-06 Finlay Slough 3-Oct-06 KOKA 235 138 1.07 -31.01 8.52 85.4 0.854 0.086 0.321 2006 FSL-02-06 Finlay Slough 3-Oct-06 KOKA 255 195 1.18 -31.59 9.64 86 0.86 0.091 0.326 2006 FSL-03-06 Finlay Slough 3-Oct-06 KOKA 255 179 1.08 -31.58 9.34 85.3 0.853 0.075 0.273 2006 FSL-06-06 Finlay Slough 3-Oct-06 KOKA 260 142 0.81 -31.90 9.32 88.1 0.881 0.092 0.252 2006 GER-44-06 Germansen River 5-Sep-06 KOKA 234 194 1.51 Partially spent -31.31 8.50 79.2 0.792 0.059 0.431 2006 GER-45-06 Germansen River 5-Sep-06 KOKA 250 173 1.11 Full of eggs -32.35 9.15 76.6 0.766 0.077 0.436 2006 GER-01-06 Germansen River 5-Sep-06 KOKA 262 196 1.09 -32.15 8.42 82 0.82 0.062 0.403 2006 GER-10-06 Germansen River 5-Sep-06 KOKA 268 213 1.11 Partially spent -33.16 9.72 78.2 0.782 0.066 0.384 2006 GER-47-06 Germansen River 5-Sep-06 KOKA 268 217 1.13 -32.42 9.44 82 0.82 0.055 0.293 2006 GER-02-06 Germansen River 5-Sep-06 KOKA 275 238 1.14 -32.27 9.75 77.7 0.777 0.078 0.354 2006 GER-05-06 Germansen River 5-Sep-06 KOKA 301 317 1.16 -32.32 10.31 79.9 0.799 0.053 0.377 2006 PEL-40-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 232 175 1.40 Partially spent -32.38 8.69 78 0.78 0.067 0.413 2006 PEL-07-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 248 203 1.33 -31.17 8.69 79 0.79 0.079 0.506 2006 PEL-16-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 254 173 1.06 Eggs -31.69 8.73 79.3 0.793 0.068 0.447 2006 PEL-31-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 260 187 1.06 Partially spent -32.52 9.85 78.6 0.786 0.049 0.329 2006 PEL-20-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 263 229 1.26 Mature -32.23 9.49 78.7 0.787 0.044 0.338 2006 PEL-01-06 Pelly Creek - 500m US of Ingenika camp 6-Sep-06 KOKA 266 276 1.47 Mature -32.06 9.37 79.4 0.794 0.071 0.456 2006 RUS-44-06 Russel Creek - 100m US of Finlay River 7-Sep-06 KOKA 233 167 1.32 Mature -31.99 8.72 76.1 0.761 0.090 0.503 2006 RUS-39-06 Russel Creek - 100m US of Finlay River 7-Sep-06 KOKA 235 170 1.31 Mature -31.84 8.80 80.2 0.802 0.068 0.417 2006 RUS-35-06 Russel Creek - 100m US of Finlay River 7-Sep-06 KOKA 241 189 1.35 Mature -31.99 8.44 78.6 0.786 0.070 0.401 2006 RUS-36-06 Russel Creek - 100m US of Finlay River 7-Sep-06 KOKA 244 197 1.36 Mature -31.52 9.17 80.6 0.806 0.094 0.456 2006 RUS-50-06 Russel Creek - 100m US of Finlay River 7-Sep-06 KOKA 253 158 0.98 Partially spent -30.96 8.85 77.7 0.777 0.106 0.477 2006 TSA-23-06 Tsaydiz Creek 6-Sep-06 KOKA 237 182 1.37 Mature -31.69 8.72 78.2 0.782 0.067 0.425 2006 TSA-18-06 Tsaydiz Creek 6-Sep-06 KOKA 238 170 1.26 Partially spent -31.43 8.26 78 0.78 0.071 0.476 2006 TSA-15-06 Tsaydiz Creek 6-Sep-06 KOKA 240 174 1.26 Ready to go -32.01 8.60 76.8 0.768 0.090 0.457 2006 TSA-03-06 Tsaydiz Creek 6-Sep-06 KOKA 243 175 1.22 Full of eggs -31.64 8.83 77.2 0.772 0.066 0.493 2006 TSA-17-06 Tsaydiz Creek 6-Sep-06 KOKA 270 234 1.19 Partially spent -31.25 9.28 79.8 0.798 0.082 0.438 2006 TSA-02-06 Tsaydiz Creek 6-Sep-06 KOKA 290 303 1.24 Partially spent -31.54 9.13 77 0.77 0.088 0.434 Length Weight Maturity Year Sample ID Catch Location Catch Date Species1 (mm) (g) Condition Comments d13C d15N moist T.Hg.dw 2 T.Hg.ww T.Se.dw 2 T.Se.ww 2015 Dav-02-15-M Davis River 16-Sep-15 BULL 440 1050 1.23 -31.43 11.35 78.5 0.215 0.537 0.115 2.260 0.486 2015 Dav-08-15-M Davis River 16-Sep-15 BULL 475 1050 0.98 -30.72 11.58 78.5 0.215 0.630 0.135 2.100 0.452 2015 Dav-09-15-M Davis River 16-Sep-15 BULL 485 1230 1.08 -31.98 11.66 78.5 0.215 0.535 0.115 1.770 0.381 2015 Dav-10-15-M Davis River 16-Sep-15 BULL 495 1050 0.87 -31.45 12.00 78.5 0.215 0.372 0.080 1.780 0.383 2015 Dav-07-15-M Davis River 16-Sep-15 BULL 520 1350 0.96 -31.02 12.13 78.5 0.215 0.788 0.169 1.830 0.393 2015 Dav-01-15-M Davis River 16-Sep-15 BULL 545 1750 1.08 -30.85 11.58 78.5 0.215 0.566 0.122 2.030 0.436 2015 Dav-03-15-M Davis River 16-Sep-15 BULL 590 2250 1.10 -30.49 11.79 78.5 0.215 0.863 0.186 2.220 0.477 2015 Dav-04-15-M Davis River 16-Sep-15 BULL 630 2350 0.94 -31.61 11.68 78.5 0.215 0.831 0.179 1.920 0.413 2015 Dav-05-15-M Davis River 16-Sep-15 BULL 740 3250 0.80 -30.51 12.74 78.5 0.215 2.680 0.576 2.410 0.518 2015 Dav-06-15-M Davis River 16-Sep-15 BULL 755 4350 1.01 -31.60 12.62 78.5 0.215 2.460 0.529 1.910 0.411 2015 ING-01-BT Ingenika River -1 18-Sep-15 BULL 710 -31.27 12.19 78.5 0.215 0.834 0.179 1.420 0.305 2015 ING-03-BT Ingenika River -1 18-Sep-15 BULL 740 -31.08 12.39 78.5 0.215 1.600 0.344 1.870 0.402 2015 ING-02-BT Ingenika River -1 18-Sep-15 BULL 780 -30.98 11.58 78.5 0.215 0.889 0.191 2.500 0.538 2015 ING-04-BT Ingenika River -2 18-Sep-15 BULL 665 -31.72 11.73 78.5 0.215 1.550 0.333 1.660 0.357 2015 ING-05-BT Ingenika River -2 18-Sep-15 BULL 730 -30.47 11.66 78.5 0.215 1.940 0.417 2.050 0.441 2015 ING-10-BT Ingenika River -3 18-Sep-15 BULL 675 -29.86 12.02 78.5 0.215 2.190 0.471 2.070 0.445 2015 ING-08-BT Ingenika River -3 18-Sep-15 BULL 730 -31.98 11.65 78.5 0.215 1.040 0.224 1.540 0.331 2015 ING-07-BT Ingenika River -3 18-Sep-15 BULL 735 -31.94 11.93 78.5 0.215 1.330 0.286 1.610 0.346 2015 ING-09-BT Ingenika River -3 18-Sep-15 BULL 763 -30.42 11.61 78.5 0.215 1.340 0.288 1.760 0.378 2015 ING-06-BT Ingenika River -3 18-Sep-15 BULL 785 -31.62 11.89 78.5 0.215 1.200 0.258 1.720 0.370 2015 Sco-05-15-M Scott Creek 19-Sep-15 BULL 340 300 0.76 -27.90 10.56 78.5 0.215 1.100 0.237 1.080 0.232 2015 Sco-01-15-M Scott Creek 18-Sep-15 BULL 462 -28.80 10.24 78.5 0.215 0.743 0.160 1.320 0.284 2015 Sco-02-15-M Scott Creek 18-Sep-15 BULL 630 -30.04 12.34 78.5 0.215 3.320 0.714 1.540 0.331 2015 Sco-04-15-M Scott Creek 19-Sep-15 BULL 710 2050 0.57 -30.12 11.69 78.5 0.215 1.770 0.381 1.430 0.307 2015 Sco-03-15-M Scott Creek 18-Sep-15 BULL 735 -30.34 12.10 78.5 0.215 4.230 0.909 1.360 0.292 2015 Sco-06-15-M Scott Creek 19-Sep-15 BULL 790 4460 0.90 -30.74 12.16 78.5 0.215 3.470 0.746 1.940 0.417 2015 RNBW-SR-9-F Thutade Lake 25-Aug-15 RNBW 111 -26.15 7.45 75.6 0.756 0.033 0.733 2015 RNBW-SR-10-F Thutade Lake 25-Aug-15 RNBW 116 -24.73 7.10 76 0.76 0.038 0.897 2015 RNBW-SR-7-F Thutade Lake 25-Aug-15 RNBW 124 -24.81 7.03 75.6 0.756 0.036 0.903 2015 RNBW-SR-8-F Thutade Lake 25-Aug-15 RNBW 128 -23.52 7.96 76.7 0.767 0.090 1.110 2015 RNBW-SR-1-F Thutade Lake 17-Aug-15 RNBW 136 -24.53 7.98 77 0.77 0.053 0.773 2015 RNBW-SR-6-F Thutade Lake 25-Aug-15 RNBW 156 -25.21 8.40 74.7 0.747 0.060 1.260 2015 RNBW-SR-2-F Thutade Lake - N of Attichika Cr. 23-Aug-15 RNBW 117 -23.82 6.90 75.6 0.756 0.030 0.841 2015 RNBW-SR-5-F Thutade Lake - N of Attichika Cr. 23-Aug-15 RNBW 128 -25.37 7.53 76.7 0.767 0.052 0.723 2015 RNBW-SR-4-F Thutade Lake - N of Attichika Cr. 23-Aug-15 RNBW 146 -24.11 8.03 75.7 0.757 0.047 0.823 2015 RNBW-SR-3-F Thutade Lake - W of Attichika Cr. 23-Aug-15 RNBW 124 -25.18 6.92 74.6 0.746 0.038 0.887

1 Species codes: KOKA = kokanee, BULL = bull trout, RNBW = rainbow trout 2 Mercury and selenium dry weight (dw) measurements for biopsy samples were converted to wet weight (ww) measures by multiplying dw value by tissue moisture percent (78.5%) Condition Outlier Red text indicates uncertainty in the data due to: 1) smudged datasheets or 2) original 2006 datasheets not provided so 2015 data was collected on thawed fish. AZIMUTH CONSULTING GROUP INC. Date Received: 16-NOV-15 ATTN: Gary Mann Report Date: 13-JAN-16 14:39 (MT) Version: FINAL # 218 - 2902 West Broadway Vancouver BC V6K 2G8

Client Phone: 604-730-1220

Certificate of Analysis Lab Work Order #: L1702897 Project P.O. #: Fish tissues Job Reference: PFWCP-15A C of C Numbers: Legal Site Desc:

Comments: Please note that, as per established Biopsy protocols, these types of samples are dried and then analyzed and reported in Dry Weight. This process is reflected for the Biopsy samples in the following data tables.

______Brent Mack, B.Sc. Account Manager [This report shall not be reproduced except in full without the written authority of the Laboratory.]

ADDRESS: 8081 Lougheed Hwy, Suite 100, Burnaby, BC V5A 1W9 Canada | Phone: +1 604 253 4188 | Fax: +1 604 253 6700 ALS CANADA LTD Part of the ALS Group A Campbell Brothers Limited Company L1702897 CONTD.... PAGE 2 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-1 L1702897-2 L1702897-3 L1702897-4 L1702897-5 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 17-AUG-15 23-AUG-15 23-AUG-15 23-AUG-15 23-AUG-15 Sampled Time Client ID RMNW-SR-1-F RMNW-SR-2-F RMNW-SR-3-F RMNW-SR-4-F RMNW-SR-5-F

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 77.0 75.6 74.6 75.7 76.7 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) <0.0060 <0.0060 <0.0060 <0.0060 <0.0060 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) 0.022 0.029 0.017 <0.010 <0.010 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 0.0023 <0.0020 <0.0020 <0.0020 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 107 104 79.0 96.1 76.2 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0130 0.0103 0.0130 0.0084 0.0108 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 0.0050 0.0044 <0.0040 0.0056 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.231 0.213 0.325 0.250 0.225 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 4.9 2.6 4.4 2.5 3.4 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 250 265 249 260 241 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.073 0.117 0.073 0.068 0.056

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 3 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-6 L1702897-7 L1702897-8 L1702897-9 L1702897-10 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 25-AUG-15 25-AUG-15 25-AUG-15 25-AUG-15 25-AUG-15 Sampled Time Client ID RMNW-SR-6-F RMNW-SR-7-F RMNW-SR-8-F RMNW-SR-9-F RMNW-SR-10-F

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 74.7 75.6 76.7 75.6 76.0 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0100 <0.0060 <0.0060 <0.0060 <0.0060 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) 0.022 0.022 0.014 0.045 <0.010 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 118 79.4 126 190 81.0 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0098 0.0140 0.0128 0.0114 0.0087 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) 0.0051 <0.0040 <0.0040 0.0060 0.0098 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.275 0.176 0.156 0.249 0.464 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 2.9 2.2 1.9 2.8 4.8 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 266 261 261 270 253 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.081 0.073 0.076 0.124 0.074

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 4 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-11 L1702897-12 L1702897-13 L1702897-14 L1702897-15 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 07-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 Sampled Time Client ID RUS-35-06 RUS-36-06 RUS-39-06 RUS-44-06 RUS-50-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 78.6 80.6 80.2 76.1 77.7 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <0.40 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0411 0.0256 0.0349 0.0409 0.0160 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) <0.010 <0.010 0.021 0.019 0.016 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 0.0024 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 0.0023 <0.0020 0.0076 0.0024 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 158 154 242 269 185 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0047 0.0040 0.0055 0.0057 0.0078 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 0.011 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) 0.0047 0.0053 0.0078 0.0052 <0.0040 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.462 0.404 0.699 0.583 0.340 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 4.2 2.79 4.8 7.4 3.6 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.0040 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 200 245 173 213 246 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.059 0.080 0.081 0.068 0.084

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 5 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-16 L1702897-17 L1702897-18 L1702897-19 L1702897-20 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 Sampled Time Client ID TSA-02-06 TSA-03-06 TSA-15-06 TSA-17-06 TSA-18-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 77.0 77.2 76.8 79.8 78.0 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <0.40 <1.0 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0214 0.0270 0.0472 0.0350 0.0154 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) 0.015 0.020 <0.010 0.030 0.023 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) 0.0013 <0.0020 <0.0020 <0.0020 0.0086 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 147 266 128 264 127 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0039 0.0058 0.0061 0.0054 0.0056 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.010 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 0.0076 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.430 0.249 0.353 0.342 0.375 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 2.78 1.7 2.5 3.3 4.3 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.0040 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 249 226 221 228 217 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.051 0.069 0.063 0.088 0.054

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 6 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-21 L1702897-22 L1702897-23 L1702897-24 L1702897-25 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 Sampled Time Client ID TSA-23-06 PEL-01-06 PEL-07-06 PEL-16-06 PEL-20-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 78.2 79.4 79.0 79.3 78.7 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <0.40 <0.40 0.41 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0301 0.0262 0.0255 0.0293 0.0165 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) <0.010 0.010 0.012 0.012 0.024 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 <0.0010 0.0049 0.0019 <0.0020 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 137 121 127 119 159 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0064 0.0049 0.0066 0.0059 0.0059 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.010 <0.010 <0.010 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 0.0058 0.0057 0.0054 <0.0040 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.352 0.524 0.562 0.405 0.327 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 2.8 4.14 5.02 3.91 2.3 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.0040 <0.0040 <0.0040 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 228 228 237 269 218 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.053 0.076 0.067 0.082 0.073

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 7 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-26 L1702897-27 L1702897-28 L1702897-29 L1702897-30 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 Sampled Time Client ID PEL-31-06 PEL-40-06 BOW-05-06 BOW-11-06 BOW-22-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 78.6 78.0 78.7 79.8 80.7 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <0.40 <1.0 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0241 0.0200 0.0249 0.0351 0.0346 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) 0.014 0.017 0.011 0.028 0.018 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) 0.0012 0.0024 <0.0020 <0.0020 0.0045 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 137 124 136 194 132 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0079 0.0048 0.0075 0.0059 0.0079 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.010 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) 0.0049 <0.0040 <0.0040 <0.0040 0.0045 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.504 0.428 0.425 0.328 0.572 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 3.32 2.9 2.9 2.6 4.9 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.0040 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 271 218 226 218 197 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.092 0.078 0.062 0.076 0.080

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 8 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-31 L1702897-32 L1702897-33 L1702897-34 L1702897-35 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 07-SEP-06 07-SEP-06 05-SEP-06 05-SEP-06 05-SEP-06 Sampled Time Client ID BOW-26-06 BOW-31-06 GER-01-06 GER-02-06 GER-05-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 77.4 75.5 82.0 77.7 79.9 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0 <1.0 <0.40 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0318 0.0493 0.0207 0.0252 0.0359 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) <0.010 0.021 0.016 0.013 0.028 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 0.0063 0.0111 0.0037 0.0019 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 134 253 138 99.2 329 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0063 0.0069 0.0071 0.0071 0.0052 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.010 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 0.0136 <0.0040 <0.0040 0.0044 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.604 0.621 0.363 0.381 0.662 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 3.8 4.2 2.2 2.5 4.01 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 <0.0040 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 245 236 264 237 215 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.058 0.074 0.051 0.065 0.062

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 9 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-36 L1702897-37 L1702897-38 L1702897-39 L1702897-40 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 05-SEP-06 05-SEP-06 05-SEP-06 05-SEP-06 21-JUN-06 Sampled Time Client ID GER-10-06 GER-44-06 GER-45-06 GER-47-06 ARC-05-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 78.2 79.2 76.6 82.0 76.7 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <0.40 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0602 0.0192 0.0234 0.0303 0.0229 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) 0.011 <0.010 0.024 <0.010 0.016 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 <0.0010 <0.0020 <0.0020 <0.0020 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 104 142 176 80.5 190 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0072 0.0047 0.0074 0.0068 0.0218 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.010 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.429 0.359 0.468 0.532 0.253 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 3.6 2.52 2.9 4.2 3.1 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.0040 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 251 264 259 199 221 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.066 0.069 0.068 0.065 0.071

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 10 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-41 L1702897-42 L1702897-43 L1702897-44 L1702897-45 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 21-JUN-06 21-JUN-06 21-JUN-06 21-JUN-06 03-OCT-06 Sampled Time Client ID ARC-07-06 ARC-08-06 ARC-33-06 ARC-49-06 FSL-02-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 73.5 77.3 74.7 75.0 86.0 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0 <1.0 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0111 0.0103 0.0091 0.0391 0.0406 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 0.038 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 159 136 228 210 218 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0193 0.0142 0.0139 0.0169 0.0042 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 0.0049 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.322 0.286 0.312 0.342 0.344 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 3.2 2.4 3.5 4.1 5.6 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 254 227 233 235 134 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.048 0.047 0.043 0.068 0.106

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 11 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-46 L1702897-47 L1702897-48 L1702897-49 L1702897-50 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 03-OCT-06 03-OCT-06 03-OCT-06 03-OCT-06 26-OCT-06 Sampled Time Client ID FSL-03-06 FSL-05-06 FSL-06-06 FSL-08-06 FIN-23-06

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 85.3 86.7 88.1 85.4 86.0 Metals Aluminum (Al)-Total (mg/kg)

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0 1.2 <1.0 Antimony (Sb)-Total (mg/kg)

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Arsenic (As)-Total (mg/kg)

Arsenic (As)-Total (mg/kg wwt) 0.0277 0.0238 0.0224 0.0357 0.0221 Barium (Ba)-Total (mg/kg)

Barium (Ba)-Total (mg/kg wwt) <0.010 0.023 0.019 0.022 0.025 Beryllium (Be)-Total (mg/kg)

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Bismuth (Bi)-Total (mg/kg)

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020 <0.0020 <0.0020 Boron (B)-Total (mg/kg)

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20 <0.20 <0.20 Cadmium (Cd)-Total (mg/kg)

Cadmium (Cd)-Total (mg/kg wwt) <0.0020 <0.0020 0.0035 <0.0020 0.0025 Calcium (Ca)-Total (mg/kg)

Calcium (Ca)-Total (mg/kg wwt) 109 172 192 160 245 Cesium (Cs)-Total (mg/kg)

Cesium (Cs)-Total (mg/kg wwt) 0.0063 0.0052 0.0039 0.0047 0.0139 Chromium (Cr)-Total (mg/kg)

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Cobalt (Co)-Total (mg/kg)

Cobalt (Co)-Total (mg/kg wwt) <0.0040 0.0041 0.0041 0.0041 0.0049 Copper (Cu)-Total (mg/kg)

Copper (Cu)-Total (mg/kg wwt) 0.274 0.206 0.212 0.339 0.229 Iron (Fe)-Total (mg/kg)

Iron (Fe)-Total (mg/kg wwt) 3.4 4.7 5.8 4.6 4.3 Lead (Pb)-Total (mg/kg)

Lead (Pb)-Total (mg/kg wwt) <0.010 <0.010 <0.010 <0.010 <0.010 Lithium (Li)-Total (mg/kg)

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10 <0.10 <0.10 Magnesium (Mg)-Total (mg/kg)

Magnesium (Mg)-Total (mg/kg wwt) 155 130 146 165 125 Manganese (Mn)-Total (mg/kg)

Manganese (Mn)-Total (mg/kg wwt) 0.051 0.069 0.078 0.154 0.068

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 12 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-51 L1702897-52 L1702897-53 L1702897-54 L1702897-55 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 26-OCT-06 26-OCT-06 26-OCT-06 16-SEP-15 16-SEP-15 Sampled Time Client ID FIN-44-06 FIN-48-06 FIN-50-06 DAV-01-15-M DAV-02-15-M

Grouping Analyte TISSUE

Physical Tests % Moisture (%) 82.7 85.7 85.6

Metals Aluminum (Al)-Total (mg/kg) <5.0 <5.0

Aluminum (Al)-Total (mg/kg wwt) <1.0 <1.0 <1.0

Antimony (Sb)-Total (mg/kg) <0.010 <0.010

Antimony (Sb)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020

Arsenic (As)-Total (mg/kg) 0.101 0.080

Arsenic (As)-Total (mg/kg wwt) 0.0339 0.0263 0.0431

Barium (Ba)-Total (mg/kg) <0.050 0.054

Barium (Ba)-Total (mg/kg wwt) <0.010 0.022 <0.010

Beryllium (Be)-Total (mg/kg) <0.010 <0.010

Beryllium (Be)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020

Bismuth (Bi)-Total (mg/kg) <0.010 <0.010

Bismuth (Bi)-Total (mg/kg wwt) <0.0020 <0.0020 <0.0020

Boron (B)-Total (mg/kg) <1.0 <1.0

Boron (B)-Total (mg/kg wwt) <0.20 <0.20 <0.20

Cadmium (Cd)-Total (mg/kg) <0.010 <0.010

Cadmium (Cd)-Total (mg/kg wwt) 0.0021 <0.0020 <0.0020

Calcium (Ca)-Total (mg/kg) 266 252

Calcium (Ca)-Total (mg/kg wwt) 102 237 114

Cesium (Cs)-Total (mg/kg) 0.0565 0.0454

Cesium (Cs)-Total (mg/kg wwt) 0.0051 0.0061 0.0076

Chromium (Cr)-Total (mg/kg) <0.20 0.91

Chromium (Cr)-Total (mg/kg wwt) <0.040 <0.040 <0.040

Cobalt (Co)-Total (mg/kg) <0.020 <0.020

Cobalt (Co)-Total (mg/kg wwt) 0.0045 0.0046 <0.0040

Copper (Cu)-Total (mg/kg) 0.77 0.94

Copper (Cu)-Total (mg/kg wwt) 0.280 0.393 0.295

Iron (Fe)-Total (mg/kg) 11.3 16.5

Iron (Fe)-Total (mg/kg wwt) 3.1 7.4 4.3

Lead (Pb)-Total (mg/kg) <0.050 <0.050

Lead (Pb)-Total (mg/kg wwt) 0.042 <0.010 <0.010

Lithium (Li)-Total (mg/kg) <0.50 <0.50

Lithium (Li)-Total (mg/kg wwt) <0.10 <0.10 <0.10

Magnesium (Mg)-Total (mg/kg) 1160 1130

Magnesium (Mg)-Total (mg/kg wwt) 191 142 159

Manganese (Mn)-Total (mg/kg) 0.235 0.289

Manganese (Mn)-Total (mg/kg wwt) 0.060 0.108 0.073

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 13 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-56 L1702897-57 L1702897-58 L1702897-59 L1702897-60 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 16-SEP-15 16-SEP-15 16-SEP-15 16-SEP-15 16-SEP-15 Sampled Time Client ID DAV-03-15-M DAV-04-15-M DAV-05-15-M DAV-06-15-M DAV-07-15-M

Grouping Analyte TISSUE

Physical Tests % Moisture (%) DLIS DLIS Metals Aluminum (Al)-Total (mg/kg) <5.0 <10 46.2 17.6 <10 Aluminum (Al)-Total (mg/kg wwt) DLIS DLIS Antimony (Sb)-Total (mg/kg) <0.010 <0.020 0.012 <0.010 <0.020 Antimony (Sb)-Total (mg/kg wwt)

Arsenic (As)-Total (mg/kg) 0.071 0.108 0.081 0.222 0.135 Arsenic (As)-Total (mg/kg wwt) DLIS Barium (Ba)-Total (mg/kg) 0.052 <0.10 0.539 0.441 0.10 Barium (Ba)-Total (mg/kg wwt) DLIS DLIS Beryllium (Be)-Total (mg/kg) <0.010 <0.020 <0.010 <0.010 <0.020 Beryllium (Be)-Total (mg/kg wwt) DLIS DLIS Bismuth (Bi)-Total (mg/kg) <0.010 <0.020 <0.010 <0.010 <0.020 Bismuth (Bi)-Total (mg/kg wwt)

Boron (B)-Total (mg/kg) 6.7 5.7 68.7 15.1 25.3 Boron (B)-Total (mg/kg wwt) DLIS DLIS Cadmium (Cd)-Total (mg/kg) <0.010 <0.020 0.030 <0.010 <0.020 Cadmium (Cd)-Total (mg/kg wwt)

Calcium (Ca)-Total (mg/kg) 262 278 463 527 853 Calcium (Ca)-Total (mg/kg wwt)

Cesium (Cs)-Total (mg/kg) 0.0604 0.084 0.0738 0.0833 0.056 Cesium (Cs)-Total (mg/kg wwt) DLIS Chromium (Cr)-Total (mg/kg) 0.26 1.03 0.85 0.26 <0.40 Chromium (Cr)-Total (mg/kg wwt) DLIS DLIS Cobalt (Co)-Total (mg/kg) <0.020 <0.040 0.025 0.023 <0.040 Cobalt (Co)-Total (mg/kg wwt)

Copper (Cu)-Total (mg/kg) 0.75 0.63 1.19 1.85 0.91 Copper (Cu)-Total (mg/kg wwt)

Iron (Fe)-Total (mg/kg) 15.2 19 110 50.4 20 Iron (Fe)-Total (mg/kg wwt) DLIS DLIS Lead (Pb)-Total (mg/kg) <0.050 <0.10 0.297 <0.050 <0.10 Lead (Pb)-Total (mg/kg wwt) DLIS DLIS Lithium (Li)-Total (mg/kg) <0.50 <1.0 <0.50 <0.50 <1.0 Lithium (Li)-Total (mg/kg wwt)

Magnesium (Mg)-Total (mg/kg) 1150 1250 1020 951 1110 Magnesium (Mg)-Total (mg/kg wwt)

Manganese (Mn)-Total (mg/kg) 0.230 0.36 1.16 0.655 0.29 Manganese (Mn)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 14 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-61 L1702897-62 L1702897-63 L1702897-64 L1702897-65 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 16-SEP-15 16-SEP-15 16-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID DAV-08-15-M DAV-09-15-M DAV-10-15-M SCO-01-15-M SCO-02-15-M

Grouping Analyte TISSUE

Physical Tests % Moisture (%) DLIS Metals Aluminum (Al)-Total (mg/kg) <10 <5.0 13 <5.0 <5.0 Aluminum (Al)-Total (mg/kg wwt) DLIS DLIS Antimony (Sb)-Total (mg/kg) <0.020 <0.010 <0.020 <0.010 <0.010 Antimony (Sb)-Total (mg/kg wwt)

Arsenic (As)-Total (mg/kg) 0.074 0.187 0.193 0.036 0.046 Arsenic (As)-Total (mg/kg wwt) DLIS Barium (Ba)-Total (mg/kg) <0.10 <0.050 0.80 0.127 0.196 Barium (Ba)-Total (mg/kg wwt) DLIS DLIS Beryllium (Be)-Total (mg/kg) <0.020 <0.010 <0.020 <0.010 <0.010 Beryllium (Be)-Total (mg/kg wwt) DLIS DLIS Bismuth (Bi)-Total (mg/kg) <0.020 <0.010 <0.020 <0.010 <0.010 Bismuth (Bi)-Total (mg/kg wwt)

Boron (B)-Total (mg/kg) 2.6 <1.0 15.1 1.2 17.8 Boron (B)-Total (mg/kg wwt) DLIS DLIS Cadmium (Cd)-Total (mg/kg) <0.020 <0.010 <0.020 <0.010 0.025 Cadmium (Cd)-Total (mg/kg wwt)

Calcium (Ca)-Total (mg/kg) 395 233 5460 802 322 Calcium (Ca)-Total (mg/kg wwt)

Cesium (Cs)-Total (mg/kg) 0.042 0.0405 0.038 0.0607 0.0716 Cesium (Cs)-Total (mg/kg wwt) DLIS Chromium (Cr)-Total (mg/kg) <0.40 0.47 0.43 0.60 0.42 Chromium (Cr)-Total (mg/kg wwt) DLIS DLIS Cobalt (Co)-Total (mg/kg) <0.040 <0.020 <0.040 0.022 <0.020 Cobalt (Co)-Total (mg/kg wwt)

Copper (Cu)-Total (mg/kg) 0.99 0.72 1.06 0.74 1.75 Copper (Cu)-Total (mg/kg wwt)

Iron (Fe)-Total (mg/kg) 12 14.1 33 13.4 15.2 Iron (Fe)-Total (mg/kg wwt) DLIS DLIS Lead (Pb)-Total (mg/kg) <0.10 <0.050 <0.10 <0.050 0.065 Lead (Pb)-Total (mg/kg wwt) DLIS DLIS Lithium (Li)-Total (mg/kg) <1.0 <0.50 <1.0 <0.50 <0.50 Lithium (Li)-Total (mg/kg wwt)

Magnesium (Mg)-Total (mg/kg) 1090 1050 639 945 861 Magnesium (Mg)-Total (mg/kg wwt)

Manganese (Mn)-Total (mg/kg) 0.20 0.310 0.85 0.471 0.426 Manganese (Mn)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 15 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-66 L1702897-67 L1702897-68 L1702897-69 L1702897-70 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 19-SEP-15 19-SEP-15 19-SEP-15 18-SEP-15 Sampled Time Client ID SCO-03-15-M SCO-04-15-M SCO-05-15-M SCO-06-15-M ING-01-BT

Grouping Analyte TISSUE

Physical Tests % Moisture (%) DLIS DLIS DLIS Metals Aluminum (Al)-Total (mg/kg) <10 <5.0 <5.0 <10 <10 Aluminum (Al)-Total (mg/kg wwt) DLIS DLIS DLIS Antimony (Sb)-Total (mg/kg) <0.020 <0.010 <0.010 <0.020 <0.020 Antimony (Sb)-Total (mg/kg wwt)

Arsenic (As)-Total (mg/kg) 0.063 0.071 0.065 0.078 0.129 Arsenic (As)-Total (mg/kg wwt)

Barium (Ba)-Total (mg/kg) 0.15 <0.050 <0.050 0.21 0.35 Barium (Ba)-Total (mg/kg wwt) DLIS DLIS DLIS Beryllium (Be)-Total (mg/kg) <0.020 <0.010 <0.010 <0.020 <0.020 Beryllium (Be)-Total (mg/kg wwt) DLIS DLIS DLIS Bismuth (Bi)-Total (mg/kg) <0.020 <0.010 <0.010 <0.020 <0.020 Bismuth (Bi)-Total (mg/kg wwt) DLIS DLIS Boron (B)-Total (mg/kg) 14.4 <1.0 <1.0 <2.0 <2.0 Boron (B)-Total (mg/kg wwt) DLIS DLIS DLIS Cadmium (Cd)-Total (mg/kg) <0.020 <0.010 <0.010 <0.020 <0.020 Cadmium (Cd)-Total (mg/kg wwt)

Calcium (Ca)-Total (mg/kg) 300 258 318 308 175 Calcium (Ca)-Total (mg/kg wwt)

Cesium (Cs)-Total (mg/kg) 0.039 0.0689 0.0585 0.089 0.055 Cesium (Cs)-Total (mg/kg wwt) DLIS Chromium (Cr)-Total (mg/kg) 0.72 0.28 0.68 0.64 <0.40 Chromium (Cr)-Total (mg/kg wwt) DLIS DLIS DLIS Cobalt (Co)-Total (mg/kg) <0.040 <0.020 <0.020 <0.040 <0.040 Cobalt (Co)-Total (mg/kg wwt)

Copper (Cu)-Total (mg/kg) 0.74 0.88 0.58 0.99 0.60 Copper (Cu)-Total (mg/kg wwt) DLIS Iron (Fe)-Total (mg/kg) 16 9.5 10.9 101 <10 Iron (Fe)-Total (mg/kg wwt) DLIS DLIS DLIS Lead (Pb)-Total (mg/kg) <0.10 <0.050 <0.050 <0.10 <0.10 Lead (Pb)-Total (mg/kg wwt) DLIS DLIS DLIS Lithium (Li)-Total (mg/kg) <1.0 <0.50 <0.50 <1.0 <1.0 Lithium (Li)-Total (mg/kg wwt)

Magnesium (Mg)-Total (mg/kg) 751 1230 1190 1170 924 Magnesium (Mg)-Total (mg/kg wwt)

Manganese (Mn)-Total (mg/kg) 0.30 0.304 0.530 0.57 0.27 Manganese (Mn)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 16 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-71 L1702897-72 L1702897-73 L1702897-74 L1702897-75 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID ING-02-BT ING-03-BT ING-04-BT ING-05-BT ING-06-BT

Grouping Analyte TISSUE

Physical Tests % Moisture (%) DLIS DLIS DLIS Metals Aluminum (Al)-Total (mg/kg) <10 <10 6.1 <10 <5.0 Aluminum (Al)-Total (mg/kg wwt) DLIS DLIS DLIS Antimony (Sb)-Total (mg/kg) <0.020 <0.020 <0.010 <0.020 <0.010 Antimony (Sb)-Total (mg/kg wwt) DLIS Arsenic (As)-Total (mg/kg) 0.244 0.140 0.152 <0.060 0.168 Arsenic (As)-Total (mg/kg wwt)

Barium (Ba)-Total (mg/kg) 0.13 0.50 0.431 0.34 0.179 Barium (Ba)-Total (mg/kg wwt) DLIS DLIS DLIS Beryllium (Be)-Total (mg/kg) <0.020 <0.020 <0.010 <0.020 <0.010 Beryllium (Be)-Total (mg/kg wwt) DLIS DLIS DLIS Bismuth (Bi)-Total (mg/kg) <0.020 <0.020 <0.010 <0.020 <0.010 Bismuth (Bi)-Total (mg/kg wwt) DLIS DLIS DLIS Boron (B)-Total (mg/kg) <2.0 <2.0 <1.0 <2.0 <1.0 Boron (B)-Total (mg/kg wwt) DLIS Cadmium (Cd)-Total (mg/kg) <0.020 0.034 <0.010 0.039 0.036 Cadmium (Cd)-Total (mg/kg wwt)

Calcium (Ca)-Total (mg/kg) 329 1500 330 573 270 Calcium (Ca)-Total (mg/kg wwt)

Cesium (Cs)-Total (mg/kg) 0.061 0.062 0.0967 0.070 0.0620 Cesium (Cs)-Total (mg/kg wwt) DLIS Chromium (Cr)-Total (mg/kg) <0.40 0.44 1.10 0.59 0.53 Chromium (Cr)-Total (mg/kg wwt) DLIS DLIS DLIS Cobalt (Co)-Total (mg/kg) <0.040 <0.040 0.020 <0.040 <0.020 Cobalt (Co)-Total (mg/kg wwt)

Copper (Cu)-Total (mg/kg) 1.21 1.68 1.79 1.48 1.21 Copper (Cu)-Total (mg/kg wwt)

Iron (Fe)-Total (mg/kg) 13 23 45.2 16 15.2 Iron (Fe)-Total (mg/kg wwt) DLIS DLIS DLIS Lead (Pb)-Total (mg/kg) <0.10 <0.10 0.062 <0.10 0.097 Lead (Pb)-Total (mg/kg wwt) DLIS DLIS DLIS Lithium (Li)-Total (mg/kg) <1.0 <1.0 <0.50 <1.0 <0.50 Lithium (Li)-Total (mg/kg wwt)

Magnesium (Mg)-Total (mg/kg) 1360 819 789 964 771 Magnesium (Mg)-Total (mg/kg wwt)

Manganese (Mn)-Total (mg/kg) 0.40 0.65 0.469 0.38 0.279 Manganese (Mn)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 17 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-76 L1702897-77 L1702897-78 L1702897-79 Description Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID ING-07-BT ING-08-BT ING-09-BT ING-10-BT

Grouping Analyte TISSUE

Physical Tests % Moisture (%) DLIS DLIS Metals Aluminum (Al)-Total (mg/kg) <5.0 <10 <5.0 <10 Aluminum (Al)-Total (mg/kg wwt) DLIS Antimony (Sb)-Total (mg/kg) 0.022 <0.020 <0.010 0.029 Antimony (Sb)-Total (mg/kg wwt)

Arsenic (As)-Total (mg/kg) 0.141 0.093 0.085 0.124 Arsenic (As)-Total (mg/kg wwt)

Barium (Ba)-Total (mg/kg) 0.635 0.67 0.274 0.72 Barium (Ba)-Total (mg/kg wwt) DLIS DLIS Beryllium (Be)-Total (mg/kg) <0.010 <0.020 <0.010 <0.020 Beryllium (Be)-Total (mg/kg wwt) DLIS DLIS Bismuth (Bi)-Total (mg/kg) <0.010 <0.020 <0.010 <0.020 Bismuth (Bi)-Total (mg/kg wwt) DLIS DLIS Boron (B)-Total (mg/kg) <1.0 <2.0 <1.0 <2.0 Boron (B)-Total (mg/kg wwt) DLIS Cadmium (Cd)-Total (mg/kg) 0.137 <0.020 <0.010 0.053 Cadmium (Cd)-Total (mg/kg wwt)

Calcium (Ca)-Total (mg/kg) 2060 3900 1740 4770 Calcium (Ca)-Total (mg/kg wwt)

Cesium (Cs)-Total (mg/kg) 0.0522 0.188 0.0857 0.133 Cesium (Cs)-Total (mg/kg wwt)

Chromium (Cr)-Total (mg/kg) 0.32 0.75 0.69 0.60 Chromium (Cr)-Total (mg/kg wwt) DLIS DLIS Cobalt (Co)-Total (mg/kg) <0.020 <0.040 <0.020 <0.040 Cobalt (Co)-Total (mg/kg wwt)

Copper (Cu)-Total (mg/kg) 1.93 0.66 9.05 2.35 Copper (Cu)-Total (mg/kg wwt)

Iron (Fe)-Total (mg/kg) 17.1 15 16.8 26 Iron (Fe)-Total (mg/kg wwt) DLIS Lead (Pb)-Total (mg/kg) 0.220 <0.10 <0.050 0.28 Lead (Pb)-Total (mg/kg wwt) DLIS DLIS Lithium (Li)-Total (mg/kg) <0.50 <1.0 <0.50 <1.0 Lithium (Li)-Total (mg/kg wwt)

Magnesium (Mg)-Total (mg/kg) 787 905 931 1050 Magnesium (Mg)-Total (mg/kg wwt)

Manganese (Mn)-Total (mg/kg) 1.02 0.34 0.444 0.93 Manganese (Mn)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 18 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-1 L1702897-2 L1702897-3 L1702897-4 L1702897-5 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 17-AUG-15 23-AUG-15 23-AUG-15 23-AUG-15 23-AUG-15 Sampled Time Client ID RMNW-SR-1-F RMNW-SR-2-F RMNW-SR-3-F RMNW-SR-4-F RMNW-SR-5-F

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0534 0.0300 0.0377 0.0467 0.0522 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2120 2270 2120 2220 2170 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 4360 4680 4020 4330 4490 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 2.31 3.09 3.34 3.13 3.19 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.773 0.841 0.887 0.823 0.723 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 223 277 185 247 219 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.109 0.107 0.085 0.070 0.034 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00561 0.00508 0.00629 0.00593 0.00778 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.033 0.024 0.032 0.031 0.022 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 4.55 4.09 4.05 7.07 3.46 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 19 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-6 L1702897-7 L1702897-8 L1702897-9 L1702897-10 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 25-AUG-15 25-AUG-15 25-AUG-15 25-AUG-15 25-AUG-15 Sampled Time Client ID RMNW-SR-6-F RMNW-SR-7-F RMNW-SR-8-F RMNW-SR-9-F RMNW-SR-10-F

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0603 0.0363 0.0898 0.0334 0.0376 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 0.240 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2250 2290 2220 2370 2320 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 4490 4620 4390 4920 4340 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 2.75 2.53 3.77 2.94 2.80 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 1.26 0.903 1.11 0.733 0.897 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 258 210 225 247 273 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.128 0.061 0.147 0.241 0.069 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00692 0.00635 0.00907 0.00494 0.00614 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) <0.020 0.031 <0.020 0.024 0.027 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 5.92 7.60 3.69 5.01 6.86 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 20 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-11 L1702897-12 L1702897-13 L1702897-14 L1702897-15 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 07-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 Sampled Time Client ID RUS-35-06 RUS-36-06 RUS-39-06 RUS-44-06 RUS-50-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0697 0.0935 0.0680 0.0896 0.106 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0040 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 0.172 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 1590 2070 1490 1630 1870 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3120 3490 2780 3110 3330 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 1.77 1.40 1.61 1.93 2.27 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.401 0.456 0.417 0.503 0.477 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 804 841 1180 799 663 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.100 0.101 0.204 0.180 0.114 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00442 0.00286 0.00443 0.00438 0.00666 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.032 0.046 0.037 0.036 0.046 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 8.06 3.82 7.80 7.68 9.24 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 21 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-16 L1702897-17 L1702897-18 L1702897-19 L1702897-20 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 Sampled Time Client ID TSA-02-06 TSA-03-06 TSA-15-06 TSA-17-06 TSA-18-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0884 0.0657 0.0899 0.0820 0.0713 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0040 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2220 1920 1800 1690 1780 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3720 4190 3360 3270 3150 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 1.88 1.90 2.04 1.78 1.82 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.434 0.493 0.457 0.438 0.476 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 857 625 593 856 689 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.111 0.151 0.076 0.179 0.107 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00480 0.00576 0.00462 0.00364 0.00329 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.039 0.037 0.033 0.028 0.041 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 3.90 8.11 7.35 9.81 5.42 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 22 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-21 L1702897-22 L1702897-23 L1702897-24 L1702897-25 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 06-SEP-06 Sampled Time Client ID TSA-23-06 PEL-01-06 PEL-07-06 PEL-16-06 PEL-20-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0671 0.0707 0.0788 0.0677 0.0436 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0040 <0.0040 <0.0040 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 1730 2060 1980 2360 1710 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3670 3500 3500 3960 3100 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 2.47 2.06 1.97 2.85 2.75 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.425 0.456 0.506 0.447 0.338 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 805 818 804 637 762 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.072 0.083 0.100 0.094 0.109 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00424 0.00419 0.00337 0.00456 0.00371 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.026 0.025 0.023 0.033 0.094 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 6.58 5.53 4.94 4.43 3.87 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 23 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-26 L1702897-27 L1702897-28 L1702897-29 L1702897-30 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 06-SEP-06 06-SEP-06 07-SEP-06 07-SEP-06 07-SEP-06 Sampled Time Client ID PEL-31-06 PEL-40-06 BOW-05-06 BOW-11-06 BOW-22-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0492 0.0669 0.0845 0.0781 0.0746 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0040 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2450 1720 1730 1650 1620 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 4000 3270 3310 3060 3250 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 3.70 1.36 2.81 2.05 2.93 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.329 0.413 0.432 0.450 0.367 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 662 809 726 912 620 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.087 0.106 0.082 0.122 0.097 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00665 0.00215 0.00562 0.00382 0.00373 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.064 0.049 0.054 0.044 0.069 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 3.75 4.42 6.91 8.63 4.66 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 24 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-31 L1702897-32 L1702897-33 L1702897-34 L1702897-35 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 07-SEP-06 07-SEP-06 05-SEP-06 05-SEP-06 05-SEP-06 Sampled Time Client ID BOW-26-06 BOW-31-06 GER-01-06 GER-02-06 GER-05-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0871 0.0967 0.0623 0.0784 0.0532 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 0.0083 <0.0080 <0.0080 <0.0040 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 1770 1610 1990 1920 1820 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3320 3360 3420 3230 3320 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 1.99 1.93 2.59 2.71 3.42 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.476 0.490 0.403 0.354 0.377 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 727 773 574 538 1010 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.082 0.164 0.097 0.071 0.156 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00461 0.00653 0.00441 0.00345 0.00270 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.087 0.060 0.044 0.059 0.043 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 5.99 8.76 4.54 6.70 9.32 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 25 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-36 L1702897-37 L1702897-38 L1702897-39 L1702897-40 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 05-SEP-06 05-SEP-06 05-SEP-06 05-SEP-06 21-JUN-06 Sampled Time Client ID GER-10-06 GER-44-06 GER-45-06 GER-47-06 ARC-05-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0657 0.0594 0.0771 0.0553 0.0473 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0040 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2000 2250 2000 1640 1880 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3460 3810 3580 3140 3200 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 2.45 2.17 2.75 3.08 1.59 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.384 0.431 0.436 0.293 0.083 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 713 846 646 704 296 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.056 0.101 0.101 0.050 0.089 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00532 0.00291 0.00340 0.00274 0.00268 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.033 0.050 0.080 0.080 0.058 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 7.19 3.69 5.81 5.70 7.36 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 26 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-41 L1702897-42 L1702897-43 L1702897-44 L1702897-45 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 21-JUN-06 21-JUN-06 21-JUN-06 21-JUN-06 03-OCT-06 Sampled Time Client ID ARC-07-06 ARC-08-06 ARC-33-06 ARC-49-06 FSL-02-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0537 0.0457 0.0553 0.0462 0.0914 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 2080 1910 1900 1920 1290 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 3450 2930 3270 3150 2310 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 1.45 1.28 1.16 1.37 1.20 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.134 0.085 0.100 0.089 0.326 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 404 300 422 325 914 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.059 0.060 0.074 0.108 0.161 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00297 0.00208 0.00210 0.00231 0.00218 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.085 0.108 0.075 <0.020 0.104 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 5.96 7.96 7.79 7.98 6.49 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 27 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-46 L1702897-47 L1702897-48 L1702897-49 L1702897-50 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 03-OCT-06 03-OCT-06 03-OCT-06 03-OCT-06 26-OCT-06 Sampled Time Client ID FSL-03-06 FSL-05-06 FSL-06-06 FSL-08-06 FIN-23-06

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg)

Mercury (Hg)-Total (mg/kg wwt) 0.0745 0.0847 0.0924 0.0864 0.134 Molybdenum (Mo)-Total (mg/kg)

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0080 <0.0080 <0.0080 <0.0080 Nickel (Ni)-Total (mg/kg)

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040 Phosphorus (P)-Total (mg/kg)

Phosphorus (P)-Total (mg/kg wwt) 1320 1260 1200 1400 1430 Potassium (K)-Total (mg/kg)

Potassium (K)-Total (mg/kg wwt) 2540 2420 2190 2980 3080 Rubidium (Rb)-Total (mg/kg)

Rubidium (Rb)-Total (mg/kg wwt) 2.42 1.45 0.674 1.67 2.69 Selenium (Se)-Total (mg/kg)

Selenium (Se)-Total (mg/kg wwt) 0.273 0.269 0.252 0.321 0.341 Sodium (Na)-Total (mg/kg)

Sodium (Na)-Total (mg/kg wwt) 893 700 748 485 1060 Strontium (Sr)-Total (mg/kg)

Strontium (Sr)-Total (mg/kg wwt) 0.064 0.133 0.128 0.128 0.173 Tellurium (Te)-Total (mg/kg)

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040 <0.0040 <0.0040 Thallium (Tl)-Total (mg/kg)

Thallium (Tl)-Total (mg/kg wwt) 0.00241 0.00170 0.00150 0.00241 0.00257 Tin (Sn)-Total (mg/kg)

Tin (Sn)-Total (mg/kg wwt) 0.081 0.113 0.175 0.044 0.119 Uranium (U)-Total (mg/kg)

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040 <0.00040 <0.00040 Vanadium (V)-Total (mg/kg)

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020 <0.020 <0.020 Zinc (Zn)-Total (mg/kg)

Zinc (Zn)-Total (mg/kg wwt) 3.88 5.99 7.09 7.39 14.5 Zirconium (Zr)-Total (mg/kg)

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 28 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-51 L1702897-52 L1702897-53 L1702897-54 L1702897-55 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 26-OCT-06 26-OCT-06 26-OCT-06 16-SEP-15 16-SEP-15 Sampled Time Client ID FIN-44-06 FIN-48-06 FIN-50-06 DAV-01-15-M DAV-02-15-M

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 0.566 0.537

Mercury (Hg)-Total (mg/kg wwt) 0.106 0.0918 0.113

Molybdenum (Mo)-Total (mg/kg) <0.040 <0.040

Molybdenum (Mo)-Total (mg/kg wwt) <0.0080 <0.0080 <0.0080

Nickel (Ni)-Total (mg/kg) <0.20 <0.20

Nickel (Ni)-Total (mg/kg wwt) <0.040 <0.040 <0.040

Phosphorus (P)-Total (mg/kg) 10700 9560

Phosphorus (P)-Total (mg/kg wwt) 1470 1380 1320

Potassium (K)-Total (mg/kg) 23300 19300

Potassium (K)-Total (mg/kg wwt) 2750 2860 2780

Rubidium (Rb)-Total (mg/kg) 17.8 15.4

Rubidium (Rb)-Total (mg/kg wwt) 1.37 2.35 1.88

Selenium (Se)-Total (mg/kg) 2.03 2.26

Selenium (Se)-Total (mg/kg wwt) 0.365 0.278 0.294

Sodium (Na)-Total (mg/kg) 1190 1080

Sodium (Na)-Total (mg/kg wwt) 919 1040 663

Strontium (Sr)-Total (mg/kg) <0.10 <0.10

Strontium (Sr)-Total (mg/kg wwt) 0.063 0.193 0.069

Tellurium (Te)-Total (mg/kg) <0.020 <0.020

Tellurium (Te)-Total (mg/kg wwt) <0.0040 <0.0040 <0.0040

Thallium (Tl)-Total (mg/kg) 0.0339 0.0293

Thallium (Tl)-Total (mg/kg wwt) 0.00233 0.00236 0.00292

Tin (Sn)-Total (mg/kg) <0.10 <0.10

Tin (Sn)-Total (mg/kg wwt) 0.068 0.070 0.040

Uranium (U)-Total (mg/kg) <0.0020 <0.0020

Uranium (U)-Total (mg/kg wwt) <0.00040 <0.00040 <0.00040

Vanadium (V)-Total (mg/kg) <0.10 <0.10

Vanadium (V)-Total (mg/kg wwt) <0.020 <0.020 <0.020

Zinc (Zn)-Total (mg/kg) 11.4 12.0

Zinc (Zn)-Total (mg/kg wwt) 5.51 9.01 7.76

Zirconium (Zr)-Total (mg/kg) <0.20 <0.20

Zirconium (Zr)-Total (mg/kg wwt) <0.040 <0.040 <0.040

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 29 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-56 L1702897-57 L1702897-58 L1702897-59 L1702897-60 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 16-SEP-15 16-SEP-15 16-SEP-15 16-SEP-15 16-SEP-15 Sampled Time Client ID DAV-03-15-M DAV-04-15-M DAV-05-15-M DAV-06-15-M DAV-07-15-M

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 0.863 0.831 2.68 2.46 0.788 Mercury (Hg)-Total (mg/kg wwt) DLIS DLIS Molybdenum (Mo)-Total (mg/kg) <0.040 <0.080 <0.040 <0.040 <0.080 Molybdenum (Mo)-Total (mg/kg wwt) DLIS Nickel (Ni)-Total (mg/kg) 0.23 <0.40 1.04 0.38 0.69 Nickel (Ni)-Total (mg/kg wwt)

Phosphorus (P)-Total (mg/kg) 9950 9450 8200 9720 9690 Phosphorus (P)-Total (mg/kg wwt)

Potassium (K)-Total (mg/kg) 19600 20200 15800 17800 18400 Potassium (K)-Total (mg/kg wwt)

Rubidium (Rb)-Total (mg/kg) 14.5 15.2 12.1 14.9 18.8 Rubidium (Rb)-Total (mg/kg wwt)

Selenium (Se)-Total (mg/kg) 2.22 1.92 2.41 1.91 1.83 Selenium (Se)-Total (mg/kg wwt)

Sodium (Na)-Total (mg/kg) 1730 1690 3300 1700 2600 Sodium (Na)-Total (mg/kg wwt) DLIS Strontium (Sr)-Total (mg/kg) <0.10 <0.20 0.46 0.27 0.38 Strontium (Sr)-Total (mg/kg wwt) DLIS DLIS Tellurium (Te)-Total (mg/kg) <0.020 <0.040 <0.020 <0.020 <0.040 Tellurium (Te)-Total (mg/kg wwt)

Thallium (Tl)-Total (mg/kg) 0.0323 0.0269 0.0231 0.0272 0.0283 Thallium (Tl)-Total (mg/kg wwt) DLIS DLIS Tin (Sn)-Total (mg/kg) <0.10 <0.20 <0.10 <0.10 <0.20 Tin (Sn)-Total (mg/kg wwt) DLIS DLIS Uranium (U)-Total (mg/kg) <0.0020 <0.0040 <0.0020 <0.0020 <0.0040 Uranium (U)-Total (mg/kg wwt) DLIS DLIS Vanadium (V)-Total (mg/kg) <0.10 <0.20 <0.10 <0.10 <0.20 Vanadium (V)-Total (mg/kg wwt)

Zinc (Zn)-Total (mg/kg) 13.1 11.2 29.3 15.1 15.5 Zinc (Zn)-Total (mg/kg wwt) DLIS DLIS Zirconium (Zr)-Total (mg/kg) <0.20 <0.40 <0.20 <0.20 <0.40 Zirconium (Zr)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 30 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-61 L1702897-62 L1702897-63 L1702897-64 L1702897-65 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 16-SEP-15 16-SEP-15 16-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID DAV-08-15-M DAV-09-15-M DAV-10-15-M SCO-01-15-M SCO-02-15-M

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 0.630 0.535 0.372 0.743 3.32 Mercury (Hg)-Total (mg/kg wwt) DLIS DLIS Molybdenum (Mo)-Total (mg/kg) <0.080 <0.040 <0.080 <0.040 <0.040 Molybdenum (Mo)-Total (mg/kg wwt) DLIS DLIS Nickel (Ni)-Total (mg/kg) <0.40 0.25 <0.40 0.68 0.73 Nickel (Ni)-Total (mg/kg wwt)

Phosphorus (P)-Total (mg/kg) 7630 8080 8530 9310 6970 Phosphorus (P)-Total (mg/kg wwt)

Potassium (K)-Total (mg/kg) 16100 17000 12700 17400 12200 Potassium (K)-Total (mg/kg wwt)

Rubidium (Rb)-Total (mg/kg) 13.4 16.2 12.6 11.3 11.5 Rubidium (Rb)-Total (mg/kg wwt)

Selenium (Se)-Total (mg/kg) 2.10 1.77 1.78 1.32 1.54 Selenium (Se)-Total (mg/kg wwt)

Sodium (Na)-Total (mg/kg) 1080 943 2600 1300 2490 Sodium (Na)-Total (mg/kg wwt) DLIS Strontium (Sr)-Total (mg/kg) <0.20 <0.10 3.19 0.72 0.56 Strontium (Sr)-Total (mg/kg wwt) DLIS DLIS Tellurium (Te)-Total (mg/kg) <0.040 <0.020 <0.040 <0.020 <0.020 Tellurium (Te)-Total (mg/kg wwt)

Thallium (Tl)-Total (mg/kg) 0.0258 0.0196 0.0205 0.0127 0.0163 Thallium (Tl)-Total (mg/kg wwt) DLIS DLIS Tin (Sn)-Total (mg/kg) <0.20 <0.10 <0.20 <0.10 <0.10 Tin (Sn)-Total (mg/kg wwt) DLIS DLIS Uranium (U)-Total (mg/kg) <0.0040 <0.0020 <0.0040 <0.0020 <0.0020 Uranium (U)-Total (mg/kg wwt) DLIS DLIS Vanadium (V)-Total (mg/kg) <0.20 <0.10 <0.20 <0.10 <0.10 Vanadium (V)-Total (mg/kg wwt)

Zinc (Zn)-Total (mg/kg) 11.8 9.4 50.3 12.5 14.4 Zinc (Zn)-Total (mg/kg wwt) DLIS DLIS Zirconium (Zr)-Total (mg/kg) <0.40 <0.20 <0.40 <0.20 <0.20 Zirconium (Zr)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 31 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-66 L1702897-67 L1702897-68 L1702897-69 L1702897-70 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 19-SEP-15 19-SEP-15 19-SEP-15 18-SEP-15 Sampled Time Client ID SCO-03-15-M SCO-04-15-M SCO-05-15-M SCO-06-15-M ING-01-BT

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 4.23 1.77 1.10 3.47 0.834 Mercury (Hg)-Total (mg/kg wwt) DLIS DLIS DLIS Molybdenum (Mo)-Total (mg/kg) <0.080 <0.040 <0.040 <0.080 <0.080 Molybdenum (Mo)-Total (mg/kg wwt) DLIS DLIS DLIS Nickel (Ni)-Total (mg/kg) <0.40 0.26 <0.20 <0.40 <0.40 Nickel (Ni)-Total (mg/kg wwt)

Phosphorus (P)-Total (mg/kg) 5090 9410 10400 10100 8240 Phosphorus (P)-Total (mg/kg wwt)

Potassium (K)-Total (mg/kg) 8840 18600 24000 20100 16300 Potassium (K)-Total (mg/kg wwt)

Rubidium (Rb)-Total (mg/kg) 12.0 15.5 12.5 17.2 14.4 Rubidium (Rb)-Total (mg/kg wwt)

Selenium (Se)-Total (mg/kg) 1.36 1.43 1.08 1.94 1.42 Selenium (Se)-Total (mg/kg wwt)

Sodium (Na)-Total (mg/kg) 2460 1220 1290 2680 1140 Sodium (Na)-Total (mg/kg wwt) DLIS Strontium (Sr)-Total (mg/kg) 0.65 <0.10 <0.10 0.20 <0.20 Strontium (Sr)-Total (mg/kg wwt) DLIS DLIS DLIS Tellurium (Te)-Total (mg/kg) <0.040 <0.020 <0.020 <0.040 <0.040 Tellurium (Te)-Total (mg/kg wwt)

Thallium (Tl)-Total (mg/kg) 0.0094 0.0217 0.0117 0.0341 0.0186 Thallium (Tl)-Total (mg/kg wwt) DLIS DLIS DLIS Tin (Sn)-Total (mg/kg) <0.20 <0.10 <0.10 <0.20 <0.20 Tin (Sn)-Total (mg/kg wwt) DLIS DLIS DLIS Uranium (U)-Total (mg/kg) <0.0040 <0.0020 <0.0020 <0.0040 <0.0040 Uranium (U)-Total (mg/kg wwt) DLIS DLIS DLIS Vanadium (V)-Total (mg/kg) <0.20 <0.10 <0.10 <0.20 <0.20 Vanadium (V)-Total (mg/kg wwt)

Zinc (Zn)-Total (mg/kg) 13.8 11.7 11.5 14.2 9.9 Zinc (Zn)-Total (mg/kg wwt) DLIS DLIS DLIS Zirconium (Zr)-Total (mg/kg) <0.40 <0.20 <0.20 <0.40 <0.40 Zirconium (Zr)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 32 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-71 L1702897-72 L1702897-73 L1702897-74 L1702897-75 Description Tissue Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID ING-02-BT ING-03-BT ING-04-BT ING-05-BT ING-06-BT

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 0.889 1.60 1.55 1.94 1.20 Mercury (Hg)-Total (mg/kg wwt) DLIS DLIS DLIS Molybdenum (Mo)-Total (mg/kg) <0.080 <0.080 <0.040 <0.080 <0.040 Molybdenum (Mo)-Total (mg/kg wwt) DLIS DLIS DLIS Nickel (Ni)-Total (mg/kg) <0.40 <0.40 0.34 <0.40 0.22 Nickel (Ni)-Total (mg/kg wwt)

Phosphorus (P)-Total (mg/kg) 10500 6900 7110 7950 6820 Phosphorus (P)-Total (mg/kg wwt)

Potassium (K)-Total (mg/kg) 22500 12700 14700 17200 13800 Potassium (K)-Total (mg/kg wwt)

Rubidium (Rb)-Total (mg/kg) 21.4 12.5 13.7 14.1 12.3 Rubidium (Rb)-Total (mg/kg wwt)

Selenium (Se)-Total (mg/kg) 2.50 1.87 1.66 2.05 1.72 Selenium (Se)-Total (mg/kg wwt)

Sodium (Na)-Total (mg/kg) 2140 1440 1460 1480 1330 Sodium (Na)-Total (mg/kg wwt)

Strontium (Sr)-Total (mg/kg) 0.33 1.24 0.27 0.58 0.28 Strontium (Sr)-Total (mg/kg wwt) DLIS DLIS DLIS Tellurium (Te)-Total (mg/kg) <0.040 <0.040 <0.020 <0.040 <0.020 Tellurium (Te)-Total (mg/kg wwt)

Thallium (Tl)-Total (mg/kg) 0.0162 0.0175 0.0276 0.0264 0.0205 Thallium (Tl)-Total (mg/kg wwt) DLIS DLIS DLIS Tin (Sn)-Total (mg/kg) <0.20 <0.20 <0.10 <0.20 <0.10 Tin (Sn)-Total (mg/kg wwt) DLIS DLIS DLIS Uranium (U)-Total (mg/kg) <0.0040 <0.0040 <0.0020 <0.0040 <0.0020 Uranium (U)-Total (mg/kg wwt) DLIS DLIS DLIS Vanadium (V)-Total (mg/kg) <0.20 <0.20 <0.10 <0.20 <0.10 Vanadium (V)-Total (mg/kg wwt)

Zinc (Zn)-Total (mg/kg) 15.6 14.7 11.2 12.8 12.7 Zinc (Zn)-Total (mg/kg wwt) DLIS DLIS DLIS Zirconium (Zr)-Total (mg/kg) <0.40 <0.40 <0.20 <0.40 <0.20 Zirconium (Zr)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 33 of 35 ALS ENVIRONMENTAL ANALYTICAL REPORT 13-JAN-16 14:39 (MT) Version: FINAL

Sample ID L1702897-76 L1702897-77 L1702897-78 L1702897-79 Description Tissue Tissue Tissue Tissue Sampled Date 18-SEP-15 18-SEP-15 18-SEP-15 18-SEP-15 Sampled Time Client ID ING-07-BT ING-08-BT ING-09-BT ING-10-BT

Grouping Analyte TISSUE

Metals Mercury (Hg)-Total (mg/kg) 1.33 1.04 1.34 2.19 Mercury (Hg)-Total (mg/kg wwt) DLIS DLIS Molybdenum (Mo)-Total (mg/kg) <0.040 <0.080 <0.040 <0.080 Molybdenum (Mo)-Total (mg/kg wwt) DLIS Nickel (Ni)-Total (mg/kg) 0.34 <0.40 2.72 0.53 Nickel (Ni)-Total (mg/kg wwt)

Phosphorus (P)-Total (mg/kg) 6500 8040 8670 10400 Phosphorus (P)-Total (mg/kg wwt)

Potassium (K)-Total (mg/kg) 12200 13400 16800 17000 Potassium (K)-Total (mg/kg wwt)

Rubidium (Rb)-Total (mg/kg) 10.2 15.5 17.1 17.5 Rubidium (Rb)-Total (mg/kg wwt)

Selenium (Se)-Total (mg/kg) 1.61 1.54 1.76 2.07 Selenium (Se)-Total (mg/kg wwt)

Sodium (Na)-Total (mg/kg) 1110 1380 1210 1630 Sodium (Na)-Total (mg/kg wwt)

Strontium (Sr)-Total (mg/kg) 1.71 2.74 1.10 3.76 Strontium (Sr)-Total (mg/kg wwt) DLIS DLIS Tellurium (Te)-Total (mg/kg) <0.020 <0.040 <0.020 <0.040 Tellurium (Te)-Total (mg/kg wwt)

Thallium (Tl)-Total (mg/kg) 0.0176 0.0113 0.0164 0.0412 Thallium (Tl)-Total (mg/kg wwt) DLIS DLIS Tin (Sn)-Total (mg/kg) <0.10 <0.20 <0.10 <0.20 Tin (Sn)-Total (mg/kg wwt) DLIS DLIS Uranium (U)-Total (mg/kg) <0.0020 <0.0040 <0.0020 <0.0040 Uranium (U)-Total (mg/kg wwt) DLIS DLIS Vanadium (V)-Total (mg/kg) <0.10 <0.20 <0.10 <0.20 Vanadium (V)-Total (mg/kg wwt)

Zinc (Zn)-Total (mg/kg) 18.0 14.9 14.6 21.2 Zinc (Zn)-Total (mg/kg wwt) DLIS DLIS Zirconium (Zr)-Total (mg/kg) <0.20 <0.40 <0.20 <0.40 Zirconium (Zr)-Total (mg/kg wwt)

* Please refer to the Reference Information section for an explanation of any qualifiers detected. L1702897 CONTD.... PAGE 34 of 35 13-JAN-16 14:39 (MT) Reference Information Version: FINAL QC Samples with Qualifiers & Comments:

QC Type Description Parameter Qualifier Applies to Sample Number(s) Duplicate Antimony (Sb)-Total DUP-H L1702897-1, -10, -11, -13, -15, -17, -18, -19, -2, -21, -3, - 4, -49, -5, -52, -53, -6, -7, -8, -9 Duplicate Barium (Ba)-Total DUP-H L1702897-1, -10, -11, -13, -15, -17, -18, -19, -2, -21, -3, - 4, -49, -5, -52, -53, -6, -7, -8, -9 Duplicate Calcium (Ca)-Total DUP-H L1702897-1, -10, -11, -13, -15, -17, -18, -19, -2, -21, -3, - 4, -49, -5, -52, -53, -6, -7, -8, -9 Duplicate Manganese (Mn)-Total DUP-H L1702897-1, -10, -11, -13, -15, -17, -18, -19, -2, -21, -3, - 4, -49, -5, -52, -53, -6, -7, -8, -9 Duplicate Strontium (Sr)-Total DUP-H L1702897-1, -10, -11, -13, -15, -17, -18, -19, -2, -21, -3, - 4, -49, -5, -52, -53, -6, -7, -8, -9 Duplicate Manganese (Mn)-Total DUP-H L1702897-14, -20, -25, -27, -28, -29, -30, -31, -32, -33, - 34, -36, -38, -39, -40, -41, -42, -43, -44, -45, -46, -47, -48, -50, -51

Qualifiers for Individual Parameters Listed: Qualifier Description

DLIS Detection Limit Adjusted: Insufficient Sample DUP-H Duplicate results outside ALS DQO, due to sample heterogeneity.

Test Method References: ALS Test Code Matrix Test Description Method Reference**

HG-DRY-MICR-CVAF-VA Tissue Mercury in Tissue by CVAFS Micro (DRY) EPA 200.3, EPA 245.7 This method is adapted from US EPA Method 200.3 "Sample Procedures for Spectrochemical Determination of Total Recoverable Elements in Biological Tissues" (1996). Tissue samples are homogenized and sub-sampled prior to hotblock digestion with nitric and hydrochloric acids, in combination with repeated additions of hydrogen peroxide. Analysis is by atomic fluorescence spectrophotometry or atomic absorption spectrophotometry, adapted from US EPA Method 245.7. HG-WET-CVAFS-N-VA Tissue Mercury in Tissue by CVAFS (WET) EPA 200.3, EPA 245.7 This method is conducted following British Columbia Lab Manual method "Metals in Animal Tissue and Vegetation (Biota) - Prescriptive". Tissue samples are homogenized and sub-sampled prior to hotblock digestion with nitric and hydrochloric acids, in combination with addition of hydrogen peroxide. Analysis is by atomic fluorescence spectrophotometry or atomic absorption spectrophotometry, adapted from US EPA Method 245.7.

HG-WET-MICR-CVAF-VA Tissue Mercury in Tissue by CVAFS Micro (WET) EPA 200.3, EPA 245.7 This method is adapted from US EPA Method 200.3 "Sample Procedures for Spectrochemical Determination of Total Recoverable Elements in Biological Tissues" (1996). Tissue samples are homogenized and sub-sampled prior to hotblock digestion with nitric and hydrochloric acids, in combination with repeated additions of hydrogen peroxide. Analysis is by atomic fluorescence spectrophotometry or atomic absorption spectrophotometry, adapted from US EPA Method 245.7. MET-DRY-MICR-HRMS-VA Tissue Metals in Tissue by HR-ICPMS Micro (DRY) EPA 200.3/200.8 Trace metals in tissue are analyzed by high resolution inductively coupled plasma mass spectrometry (HR-ICPMS) modified from US EPA Method 200.8, (Revision 5.5). The sample preparation procedure is modified from US EPA 200.3. Analytical results are reported on dry weight basis.

Method Limitation: This method employs a strong acid/peroxide digestion, and is intended to provide a conservative estimate of bio-available metals. Near complete recoveries are achieved for most toxicologically important metals, but elements associated with recalcitrant minerals may be only partially recovered. MET-WET-CCMS-N-VA Tissue Metals in Tissue by CRC ICPMS (WET) EPA 200.3/6020A This method is conducted following British Columbia Lab Manual method "Metals in Animal Tissue and Vegetation (Biota) - Prescriptive". Tissue samples are homogenized and sub-sampled prior to hotblock digestion with nitric and hydrochloric acids, in combination with addition of hydrogen peroxide. Instrumental analysis is by collision cell inductively coupled plasma - mass spectrometry (modified from EPA Method 6020A).

Method Limitation: This method employs a strong acid/peroxide digestion, and is intended to provide a conservative estimate of bio-available metals. Near complete recoveries are achieved for most toxicologically important metals, but elements associated with recalcitrant minerals may be only partially recovered.

MET-WET-MICR-HRMS-VA Tissue Metals in Tissue by HR-ICPMS Micro (WET) EPA 200.3/200.8 Trace metals in tissue are analyzed by high resolution inductively coupled plasma mass spectrometry (HR-ICPMS) modified from US EPA Method 200.8, (Revision 5.5). The sample preparation procedure is modified from US EPA 200.3. Analytical results are reported on wet weight basis.

Method Limitation: This method employs a strong acid/peroxide digestion, and is intended to provide a conservative estimate of bio-available metals. Near complete recoveries are achieved for most toxicologically important metals, but elements associated with recalcitrant minerals may be only partially recovered. MOISTURE-TISS-VA Tissue % Moisture in Tissues ASTM D2974-00 Method A L1702897 CONTD.... PAGE 35 of 35 13-JAN-16 14:39 (MT) Reference Information Version: FINAL

This analysis is carried out gravimetrically by drying the sample at 105 C for a minimum of six hours.

** ALS test methods may incorporate modifications from specified reference methods to improve performance. The last two letters of the above test code(s) indicate the laboratory that performed analytical analysis for that test. Refer to the list below:

Laboratory Definition Code Laboratory Location

Chain of Custody Numbers: GLOSSARY OF REPORT TERMS Surrogate - A compound that is similar in behaviour to target analyte(s), but that does not occur naturally in environmental samples. For applicable tests, surrogates are added to samples prior to analysis as a check on recovery. mg/kg - milligrams per kilogram based on dry weight of sample. mg/kg wwt - milligrams per kilogram based on wet weight of sample. mg/kg lwt - milligrams per kilogram based on lipid-adjusted weight of sample. mg/L - milligrams per litre. < - Less than. D.L. - The reported Detection Limit, also known as the Limit of Reporting (LOR). N/A - Result not available. Refer to qualifier code and definition for explanation.

Test results reported relate only to the samples as received by the laboratory. UNLESS OTHERWISE STATED, ALL SAMPLES WERE RECEIVED IN ACCEPTABLE CONDITION. Analytical results in unsigned test reports with the DRAFT watermark are subject to change, pending final QC review.

SINLAB INTERPRETATION GUIDE For further information please visit our website: http://www.unb.ca/research/institutes/cri/sinlab/

Instrumentation

Continuous Flow-Isotope Ratio Mass Spectrometry (CF-IRMS) is used for stable isotope analysis of δ13C, δ 15N and δ 2H. The SINLAB currently operates the following mass spectrometer/conflo combinations: • Delta Plus – Conflo II • DeltaPlus XP – Conflo III • Delta V Plus – Conflo IV

(All manufactured by Thermo Finnigan; Bremen, Germany)

Carbon & Nitrogen Methodology

Dried, ground and homogeneous samples are weighed into tin capsules and analyzed for δ 13C and δ 15N by an Elemental Analyzer (EA) coupled to one of the IRMS/Conflo combinations listed above. Samples are introduced into the EA via an autosampler where complete combustion occurs in the presence of oxygen to generate CO2 and nitrogen oxide (NxOx) gases. Combustion occurs in a quartz tube filled with chromium oxide and silvered cobaltous oxide. A second quartz tube filled with fine copper wire is used for the reduction of nitrogen oxides (NxOx) to N2 gas. Gas Chromatography (GC) is used to separate CO2 and N2 peaks with helium as a carrier gas. A water trap of magnesium perchlorate & silica chips is located before the GC column to remove water.

The SINLAB currently utilizes three elemental analyzers for δ 13C and δ 15N analyses.

Elemental Analyzer Autosampler Combustion Reduction GC Length GC Temperature Temperature Temperature CE NC2500 AS200 1050ºC 650ºC 4m 50ºC (Carlo Erba; Milan, Italy) Costech 4010 Zero Blank 1000ºC 650oC 3m 40ºC (Costech; California, USA) CE NA1500 PN120 1020oC 650oC 3m 50oC (Carlo Erba; Milan, Italy)

Stable isotope measurements are reported as isotope delta δ in parts per thousand (‰) relative to the international standard: Vienna Pee Dee Belemnite (VPDB) for carbon, and atmospheric air (AIR) for nitrogen. Isotope values are normalized using secondary standards: NICOTINAMIDE, BLS, and MLS for animal tissues; and CMS, AQM, SPL and EPS for sediments and plant material. All of these standards were calibrated against IAEA standards. See below for standard descriptions.

1 Hydrogen Methodology

Samples are weighed into silver capsules and loaded into a Costech Zeroblank autosampler. Samples are converted to hydrogen (H2) gas by pyrolysis using a Thermo-Finnigan High Temperature Conversion Elemental Analyzer (TC/EA). Pyrolysis occurs in a ceramic tube lined with a glassy carbon reactor and filled with glassy carbon chips at a temperature of 1400ºC. Helium is used as the carrier gas and a 1.5m GC column held at 100ºC separates H2 sample gas and other interfering gases produced

Stable-hydrogen isotope (δ 2H) measurements for keratin tissues are normalized to the international standard VSMOW (Vienna Standard Mean Ocean Water). We determine the non-exchangeable δ 2H of samples using the comparative equilibration approach (Wassenaar and Hobson 2003) with two secondary keratin standards (EC1 and EC2). These standards were previously calibrated to account for the H exchangeability between the H atoms of ambient water vapor and keratin (Wassenaar and Hobson 2000, 2003). This technique requires that samples along with these standards of known H isotope ratios are left to exchange with local atmospheric hydrogen for 72 hours prior to analysis. See below for standard descriptions.

Standards

Secondary Standards – These are SINLAB working standards calibrated against and traceable to IAEA primary standards (CH6, CH7, N1, and N2). These standards are subjected to round robin testing for verification as a part of our QA/QC protocol.

NICOTINAMIDE = commercially available pure compound Batch number 182979 (May 2015-present) 13 δ C (VPDB) = –34.57 ‰ +/- 0.13 15 δ N (AIR) = 0.02 ‰ +/- 0.10

BLS = Bovine Liver Standard developed by SINLAB 13 δ C (VPDB) = –18.76 ‰ +/- 0.14 15 δ N (AIR) = 7.17 ‰ +/- 0.17

MLS = Muskellunge muscle standard developed by SINLAB 13 δ C (VPDB) = –22.30 ‰ +/- 0.18 15 δ N (AIR) = 14.00 ‰ +/- 0.11

CMS = Corn Meal Standard developed by SINLAB 13 δ C (VPDB) = –13.25 ‰ +/- 0.11 15 δ N (AIR) = 4.42 ‰ +/- 0.12

AQM = Aquatic Moss Standard developed by SINLAB 13 δ C (VPDB) = -35.08 ‰ +/- 0.15 15 δ N (AIR) = 16.14 ‰ +/- 0.07

EPS = Ephedra Plant Standard developed by SINLAB 13 δ C (VPDB) = -30.96 ‰ +/- 0.09 15 δ N (AIR) = 0.35 ‰ +/- 0.12

2 SPL = Spirulina standard developed by SINLAB 13 δ C (VPDB) = -24.97 ‰ +/- 0.12 15 δ N (AIR) = 12.94 ‰ +/- 0.09

EC1 = caribou hoof keratin standard- Environment Canada, Saskatoon, Canada 2 δ H (VSMOW) = –197 ‰ +/- 1.8

EC2 = kudu horn keratin standard - Environment Canada, Saskatoon, Canada 2 δ H (VSMOW) = –54.1 ‰ +/- 0.6

Check Standards – These standards are analyzed in each analytical run as part of SINLAB’s QA/QC protocol to assess the analytical accuracy.

ACETANILIDE = commercially available pure compound 13 Batch 2880 (Feb 2010 – Apr 2011) - δ C (VPDB) = –27.87 ‰ +/- 0.12 15 δ N (AIR) = –2.05 ‰ +/- 0.13

13 Batch 149699 (Apr 2011-Aug 2012) - δ C (VPDB) = –31.59 ‰ +/- 0.12 15 δ N (AIR) = –2.32 ‰ +/- 0.23

13 Costech (Aug 2012 – Present) - δ C (VPDB) = –33.81 ‰ +/- 0.14 15 δ N (AIR) = –0.92 ‰ +/- 0.23

N2 = ammonium sulfate – Primary standard certified by IAEA. 15 δ N (AIR) = 20.3 ‰ +/- 0.14

CH7 = polyethylene foil – Primary standard certified by IAEA. 13 δ C (VPDB) = –32.15 ‰ +/- 0.10

PROTEIN = casein – Certified by Elemental Microanalysis Ltd. 13 δ C (VPDB) = –26.98 ‰ +/- 0.13 15 δ N (AIR) = 5.94 ‰ +/- 0.08

HIGH ORGANIC SEDIMENT= Certified by Elemental Microanalysis Ltd. 13 δ C (VPDB) = –26.27 ‰ +/- 0.15 15 δ N (AIR) = 4.42 ‰ +/- 0.29

SORGHUM FLOUR= Certified by Elemental Microanalysis Ltd. 13 δ C (VPDB) = –13.68 ‰ +/- 0.19 15 δ N (AIR) = 1.58 ‰ +/- 0.15

PEACH LEAF = NIST 1547 peach leaves - not certified 13 δ C (VPDB) = –26.17 ‰ +/- 0.08 15 δ N (AIR) = 1.94 ‰ +/- 0.12

KERATIN STANDARD = Keratin powder purchased from Spectrum. B/N SJ1400– not certified 2 δ H (VSMOW) = –122 ‰ +/- 2 3 Column Headings

CLIENT ID = ID code assigned to sample by the client.

SINLAB ID = ID code assigned to the client’s samples; starting with the year, each client is given a two or three letter identifier and samples numbered sequentially; ex, 15ABC 001.

Date = date sample was analyzed.

Position = position in the analytical run for that particular day; samples are weighed into 96-well ELISA trays, a typical animal tissue run will consist of approximately 73 samples, 22 standards, and 1 blank.

Weight = weight of the tissue analyzed; animal tissues are weighed at 1.000 ± 0.100 milligrams and plant tissues are weighed at 3.100 ± 0.100 milligrams for C and N isotope analysis. Keratin tissues are weighed at 0.200 ± 0.020mg for H isotope analysis.

CO2 ampl = the relative amount of CO2 gas measured by the mass spectrometer in volts (V), a function of the weight of tissue used and the total amount of carbon (%C) it contains.

N2 ampl = the relative amount of N2 gas measured by the mass spectrometer in volts (V), a function of the weight of tissue used and the total amount of nitrogen (%N) it contains.

H2 ampl = the relative amount of H2 gas measured by the mass spectrometer in volts (V), a function of the weight of tissue used and the total amount of hydrogen (%H) it contains.

δ 13C = the relative isotope ratio difference between the sample and the international standard (VPDB) according to the formula: 13 13 12 δ C = [(Rsample/Rstandard)-1]*1000 where R is the isotopic ratio of the heavy to light ( C/ C)

δ 15N = the relative isotope ratio difference between the sample and the international standard (AIR) according to the formula: 15 15 14 δ N = [(Rsample/Rstandard)-1]*1000 where R is the isotopic ratio of the heavy to light ( N/ N)

δ 2H = the relative isotope ratio difference between the sample and the international standard (VSMOW) according to the formula: 2 2 1 δ H = [(Rsample/Rstandard)-1]*1000 where R is the isotopic ratio of the heavy to light ( H/ H)

%C = percent of carbon in the sample by weight; %N = percent of nitrogen in the sample by weight; C/N = ratio of carbon to nitrogen in the sample; simple division of %C by %N.

%H= percent of hydrogen in the sample by weight.

4

Comment Codes

NR = no repeat; not enough sample tissue to allow another analysis

No drop = equipment malfunction wherein autosampler fails to turn; often leads to a “double-up” with the following sample

Double-up = two samples drop together

LR = lipid-rich. Samples may contain high lipid content according to the C/N ratio (Logan et al. 2008)

Whole bug = individual analyzed without grinding

1/4, 1/8, 1/16, 1/32 = indicates the size of a filter paper sample that was cut into a “pie-slice” for analysis

Scraped from paper = filtered material was scraped from the top of filter rather than analyzed as a “pie slice”

LE = Lipid extracted, a common technique to remove lipids from tissues such as liver, eggs, and muscle of some fishes. Lipids have different δ 13C than proteins and carbohydrates.

AT = Acid treated, a common technique to remove carbonates (that have different δ 13C values than organic tissues) from organisms such as crustaceans.

Colours

Gray shading = repeated sample as part of regular QA/QC routine (four of every 73 samples) Red text = highlights low amplitude peaks or a poor repeat

Please address any questions about this document to:

Dr. Brian Hayden Science Manager, Stable Isotopes in Nature Laboratory (SINLAB), Canadian Rivers Institute, University of New Brunswick, Fredericton, New Brunswick, Canada, E3B 5A3 email: [email protected] phone: 506.451.6892 (office), 506.453.4967 (lab) fax: 506.453.3583 http://www.unb.ca/research/institutes/cri/sinlab/

5 References

Logan, J.M., Jardine, T.D., Miller, T.J., Bunn, S.E., Cunjak, R.A., and Lutcavage, M.E. 2008. Lipid corrections in carbon and nitrogen stable isotope analyses: comparison of chemical extraction and modelling methods. Journal of Animal Ecology 77(4): 838-846.

Wassenaar, L.I., and Hobson, K.A. 2000. Improved method for determining the stable-hydrogen isotopic composition (δD) of complex organic materials of environmental interest. Environmental Science and Technology 34(11): 2354-2360.

Wassenaar, L.I., and Hobson, K.A. 2003. Comparative equilibration and online technique for determination of non-exchangeable hydrogen of keratins for use in animal migration studies. Isotopes in Environmental and Health Studies 39(3): 211-217.

6 Williston Reservoir Watershed – 2015 Reconnaissance Fish Mercury Sampling Program

APPENDIX C – KOKANEE FIELD PHOTOS HIGHLIGHTING RANGE IN MORPHOLOGY

20 June 2016 Appendix C: Kokanee field photos highlighting range in morphology

Kokanee caught in Russel Creek, Sept 2006 Kokanee caught in Pelly Creek, Sept 2006

Kokanee caught in Arctic Lake, June 2006 Kokanee caught in Finlay Slough, Sept 2006