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Tyler Mehler 1 , Jing You 2 , Jon Maul 3 and Michael Lydy 1

Identification of the Causes of Sediment-Associated Toxicity in the Illinois River Complex Using a Sediment-TIE Approach. Tyler Mehler 1 , Jing You 2 , Jon Maul 3 and Michael Lydy 1

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Tyler Mehler 1 , Jing You 2 , Jon Maul 3 and Michael Lydy 1

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  1. Identification of the Causes of Sediment-Associated Toxicity in the Illinois River Complex Using a Sediment-TIE Approach Tyler Mehler1, Jing You2, Jon Maul3 and Michael Lydy1 1Fisheries and Illinois Aquaculture and Department of Zoology, Southern Illinois University, Carbondale, Illinois, USA 2State Key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, China 3The Institute of Environmental and Human Health, Department of Toxicology, Box 41163, Texas Tech University, Lubbock, Texas, USA ISTC seminar: 9/9/09

  2. What is a TIE? As defined by the EPA (2007): The Toxicity Identification Evaluation approach “is to use physical/chemical manipulations of a sample to isolate or change the potency of different groups of toxicants potentially present in a sample”. Contaminated w/ non-polar organics X X X X X X X X X Amended for ammonia Amended for non-polar organics Unamended Amended for metals Amended

  3. Matrix Choice Sediment grain Pore water usgs.gov • Issues with pore water TIEs: • Bioavailability • Ingestion • Water quality parameters • Environmental Realistic?

  4. Conducting a Toxicity Identification Evaluation (TIE) STEP 1 SITE SAMPLING STEP 2 SCREENING TOXICITY TEST STEP 3 PHASE I: CHARACTERIZATION Ammonia (Zeolite) Cationic Metals (Resin-Tech SIR 300) X Nonpolar Organics (PCC) Unamended Amended STEP 4 PHASE II: IDENTIFICATION Ammonia (Ammonia Probe) Cationic metals (NAD & FAAS) Nonpolar Organics (ASE & GC/HPLC) concentration of contaminant LC50 of that contaminant Toxic Unit (TU) = U.S. EPA 2007 Whole sediment TIE guidelines

  5. Objectives • Identify toxic sites throughout the Illinois River Complex • Identify the contaminant classes (ammonia, metals, non-polar organics) that attribute to the toxicity of those sites using a whole-sediment TIE test • Evaluate the temporal and spatial trends in correlation to the toxicity of those sites • Examine the difference between TIE methodologies and the test organisms used • Compare past and present TIE research on the IRC

  6. Conducting a Toxicity Identification Evaluation (TIE) STEP 1 SITE SAMPLING SITE SAMPLING STEP 2 SCREENING TOXICITY TEST STEP 3 PHASE I: CHARACTERIZATION Ammonia (Zeolite) Cationic Metals (Resin-Tech SIR 300) Nonpolar Organics (PCC) STEP 4 PHASE II: IDENTIFICATION Ammonia (Ammonia Probe) Cationic metals (NAD & FAAS) Nonpolar Organics (ASE & GC/HPLC)

  7. Sampling Methods • 24 sites chosen with consultation of ISTC • 2.5 kg was collected from each site • Water samples from each site were also retrieved and water quality measurements for each site taken • Hardness emulated • Total pore water ammonia was analyzed upon arrival at SIUC • Sediments and water samples were analyzed at SIUC Fisheries and Illinois Aquaculture Center • Samples were taken in summer 07’, fall 07’, winter 07-08’, spring 08’ and again in summer 08’ 17

  8. SitesRivermile 17 St. Louis Carbondale X

  9. Conducting a Toxicity Identification Evaluation (TIE) STEP 1 SITE SAMPLING STEP 2 SCREENING TOXICITY TEST SCREENING TOXICITY TEST STEP 3 PHASE I: CHARACTERIZATION Ammonia (Zeolite) Cationic Metals (Resin-Tech SIR 300) Nonpolar Organics (PCC) STEP 4 PHASE II: IDENTIFICATION Ammonia (Ammonia Probe) Cationic metals (NAD & FAAS) Nonpolar Organics (ASE & GC/HPLC)

  10. Screening Toxicity Tests • 10-d bioassays (U.S. EPA) in flow-thru system with three water changes per day (100 ml per change) • 10 H. azteca (14 to 21-d old) per 300 ml beaker, 6 replicates per site • Control: Touch of Nature (TON) hydrated soil – Carbondale, IL • Amendment Reference: Lower Peoria Lake (LPL) • Statistical Analysis: Dunnett’s Multiple Comparison Test

  11. Summer 07’ Results: Screening Toxicity Tests Halstead Touch of Nature Moore’s Towhead Spring Lake Wildlife Area Pekin Wesley Upper Lower Peoria Lake LPL Dredge Goose Lacon Mudd Hennepin Down River Hennenpin Power Plant DuPue Marseilles DuPage CS305 SS308 Stony Creek SS315 SS317 SRCALRR Sites that were significantly different from controls (p<0.05) and were chosen for seasonal analysis.

  12. Conducting a Toxicity Identification Evaluation (TIE) STEP 1 SITE SAMPLING STEP 2 SCREENING TOXICITY TEST STEP 3 PHASE I: CHARACTERIZATION PHASE I: CHARACTERIZATION Ammonia (Zeolite) Cationic Metals (Resin-Tech SIR 300) Nonpolar Organics (PCC) STEP 4 PHASE II: IDENTIFICATION Ammonia (Ammonia Probe) Cationic metals (NAD & FAAS) Nonpolar Organics (ASE & GC/HPLC)

  13. Phase I: Characterization 20% (12 g) Zeolite 20% (12 g) Unamended (sand) 4 -d static test 10 H. azteca 6 reps per treatment 25% (15 g) 10-d flow-thru test RT SIR 300 HP 15% (9 g) PCC 25% (15 g) Unamended (sand)

  14. Summer 2007 Results: Phase I Unamended (sand) Organics (PCC) TON LPL SS308 Halstead CS305 Stny Crk SRCALRR SS315 DuPage TOXIC SITES • The addition of zeolite (ammonia) and Resin-Tech SIR 300 (metals) showed no significant differences in comparison to the unamended sediment.

  15. Conducting a Toxicity Identification Evaluation (TIE) STEP 1 SITE SAMPLING STEP 2 SCREENING TOXICITY TEST STEP 3 PHASE I: CHARACTERIZATION Ammonia (Zeolite) Cationic Metals (Resin-Tech SIR 300) Nonpolar Organics (PCC) STEP 4 PHASE II: IDENTIFICATION PHASE II: IDENTIFICATION Ammonia (Ammonia Probe) Cationic metals (NAD & FAAS) Nonpolar Organics (ASE & GC/HPLC)

  16. Phase II: Identification Nonpolar Organic Toxicants PAHs:acenaphthene, acenapthylene, anthracene, chrysene, fluoranthene, fluorene, naphthalene, phenanthrene, pyrene, benzo[a]anthracene, benzo[b]fluoranthrene, benzo[k]fluoranthene, benzo[a]pyrene, benzo[g,h,i]perylene, dibenzo[a,h]anthracene and indeno[1,2,3-cd]pyrene PCBs:Congeners: 8, 18, 28, 31, 43, 44, 48, 49, 52, 66, 70, 86, 87, 95, 97, 99, 101, 105, 110, 114, 118, 123, 126, 128, 138, 153, 156, 157, 167, 169, 170, 174, 180, 183, 187, 189, 194, 195, 200, 201, 203 and 206. OCPs:alpha-BHC, beta-BHC, gamma-BHC, delta-BHC, p,p’-DDE, p,p’-DDD, p,p’-DDT, aldrin, gamma-chlordane, alpha-chlordane, diedrin, endrin, endrin aldehyde, endrin ketone, endosulfan I, endosulfan II, endosulfan sulfate, heptachlor, heptachlor epoxide and methoxychlor. OP/Pyrethroids:chlorpyrifos, permethrin, lambda-cyhalothrin, cypermethrin, esfenvalerate, deltamethrin, cyfluthrin, bifenthrin. Heavy Metals Cu2+, Ni2+, Cr6+, Pb2+, Zn2+, Cd2+ Ammonia NH4+, NH3

  17. The reasons we analyzed total ammonia: • It’s commonly performed in standard TIE methods • Allows comparisons in pore water ammonia concentrations between past and present studies (Sparks and Ross 1992 – Concentrations measured as total ammonia) • Allows comparisons in pore water ammonia concentrations among sites (since water quality characteristics differed among sites) • Difficult to account for drifting pHs or changing temperature throughout studies

  18. Summer 2007 Phase II: Identification BRL – 1 µg/kg Low TU = Low Toxicity High TU= High Toxicity

  19. Summer 2007 Conclusions • Phase I findings strongly suggests that non-polar organics are the problem, with Phase II findings further suggesting that PAHs were at high concentrations to cause the noted toxicity. • What about the other seasons?

  20. SUMMER 07’ SUMMER 08’ Is PCC always effective? • 46% of sites (in all seasons) were characterized with PCC Unamended (sand) Organics (PCC) • Affect on PCC binding capability? • Organics higher affinity for UCM? • Causes toxicity itself? % Unresolved Complex Matrix (UCM)

  21. Phase II: Spatial and temporal variation Total Pore Water Ammonia Summer 2007 Fall 2007 Winter 2007-2008 Spring 2008 Summer 2008 mg N/L Calumet Sag Channel Chicago Sanitary and Shipping Canal Total Cationic Metals µg/g dry wt Concentration of Contaminant Total PAHs 6.0 mg/g OC 3.0 LPL SS315 SS308 SRCALRR CS305 Stony Creek Halstead

  22. Spatial Trends: Ammonia

  23. Spatial Trends: Ammonia Municipal Waste Plant SS315 Total Ammonia >400 mg N/L Courtesy of www.flashearth.com

  24. Sparks and Ross (1992) • Gradient of increased toxicity associated with the total ammonia concentration • Ammonia the primary source of toxicity in the Illinois River Complex • Patches of toxicity occurring due to PAHs

  25. A Comparison Study: • Determine differences between pore water TIE testing and whole-sediment TIE testing • Determine differences between test organisms (H. aztecaand C. dubia) • While still comparing past and present research Two sites being evaluated: SS315 – highest ammonia concentrations SS308 – highest PAH concentrations VS VS

  26. Phase I: Pore Water Characterization Diluted by 50% Unamended 2-d static test 1-d static test Zeolite 5 H. azteca 10 C. dubia 8 reps per treatment SPE C18

  27. Phase I: Whole Sediment Characterization 4-d static test Zeolite Unamended 10-d flow-thru test PCC 10 H. azteca 10 C. dubia 8 reps per treatment Zeolite Unamended 2-d static test PCC

  28. Comparing Methodologies: Ammonia Whole Sediment TIE PHASE I: Pore Water TIE 2.56 0.27 Predicted TUs for H. azteca PHASE II: SS315 Ammonia Concentrations (mg N/L) 359 mg N/L 37.9 mg N/L

  29. Comparing Methodologies: Non-polar Organics PHASE I: Whole-Sediment TIE Pore Water TIE • The affects of: • UCM • Black carbon • ingestion, adsorption • DOC • Glassware binding 0.52 1.81 TUs for H. azteca PHASE II: SS308 ∑PAH Concentrations: 1953 µg/L 4405 µg/g oc

  30. Comparing Species Sensitivity/Susceptibility LC50 Total Ammonia: H. azteca  140 mg N/L (4-d)a  47.25 mg N/L (2-d)b C. dubia LC50 Fluoranthene (PAH): H. azteca  30.6 µg/L (10-d)c  102.6 µg/L (10-d)c C. dubia a – Ankley et al. 1995 b – extrapolated from Bailey et al. 2001 c – Suedel and Rodgers, Jr. 1996 • Species Sensitivity ≠ Species Susceptibility • Body Size /Age (Life Stage) • Physiology/Feeding Behavior • Niche

  31. Conclusions • Toxic sites were identified on the IRC for future risk assessment & mitigation • Rm 277 (DuPage) Calumet Sag Channel, Chicago Sanitary and Shipping Canal

  32. Conclusions • PAHs and the associated oils and grease were identified as the sources of the noted toxicity, however ammonia was elevated at SS315

  33. Conclusions • Little temporal variation was noted in toxicity and in concentrations • However, spatial trends were found in toxicity especially concerning ammonia

  34. Conclusions • Which TIE approach is better and where are TIEs headed? • Is the IRC a healthy system ?

  35. Acknowledgements Sampling Crew: Ed Workman, Mandy Rothert, Liz Tripp, Heather Foslund A special thanks goes to SETAC (Student Exchange Program) and Teresa Norberg-King and the rest of the EPA Duluth Lab. Fisheries and Aquaculture Center and Dept. of Zoology staff and students Funding:

  36. For more information: Mehler WT, Maul JD, You J, and MJ Lydy. 2009. Identifying the causes of sediment-associated contamination in the Illinois River using a whole-sediment Toxicity Identification Evaluation (TIE). Environmental Toxicology and Chemistry. In Press. Mehler WT, You J, Maul JD, and MJ Lydy. 2009. Comparative analysis of whole sediment and pore water Toxicity Identification Evaluation (TIE) techniques for ammonia and non-polar organic contaminants. Chemosphere. In Review.

  37. Questions?

  38. Evaluating Ammonia SS315 overlying water Total ammonia – 37.9 mg N/L (TU = 0.29) Un-ionized ammonia – 0.584 mg/L (TU = 0.27) SS315 pore water Total ammonia – 359 mg N/L (TU = 2.56) Un-ionized ammonia – 11.2 mg/L (TU = 5.19)

  39. Sparks and Ross (1992) • Gradient of increased toxicity associated with the total ammonia concentration • Ammonia was the primary source of toxicity in the Illinois River Complex • Patches of toxicity occurring due to PAHs • The beginning of a general recovery of the Illinois River Complex

  40. Sparks and Ross 1992 • Gradient of increased toxicity associated with the total ammonia concentration • Ammonia the primary source of toxicity in the Illinois River Complex • Patches of toxicity occurring due to PAHs • The beginning of a general recovery of the Illinois River Complex ?

  41. Questions?

  42. Conclusions: • Differences in past and present TIE studies is attributed to the differences in methodologies and perhaps on a lesser note test organism choice. • Which test organism is better? • Realistic Test Organism? • Using Historic Test Organism? • Which TIE is better and where are TIEs headed?

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