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Analysis of the Codorus Creek

Analysis of the Codorus Creek. Quantitative Analytical Chem. Fall 2002. Agenda. Background Purpose of study Sampling scheme Major Polluters Clean-up Acts Chloride Analysis Sulfates. Agenda Continued. Sulfites Calcium and Magnesium Nitrates Various Metals (silver, mercury, and lead).

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Analysis of the Codorus Creek

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  1. Analysis of the Codorus Creek Quantitative Analytical Chem. Fall 2002

  2. Agenda • Background • Purpose of study • Sampling scheme • Major Polluters • Clean-up Acts • Chloride Analysis • Sulfates

  3. Agenda Continued • Sulfites • Calcium and Magnesium • Nitrates • Various Metals (silver, mercury, and lead)

  4. Codorus Creek Study • Purpose of Study • Use various analytical techniques from previous methods • Titrimetric, gravimetric, and UV-Vis • Determine amounts of analyte in East and West Branches and Main Branch of Codorus Creek

  5. Where Our Water Comes From • http://www.yorkwater.com/

  6. Sampling Scheme • Sampled above and below PH Glatfelter (West Branch) • 616 Bridge • Sampled above and below Indian Rock Dam (East Branch) • Ridge View Rd. • Reynolds Mill Rd. • Sampled from the South Branch • Sampled from Waterway Bar and Grill, Philadelphia St. • Sampled from Indian Rock Campground

  7. Sampling Scheme Continued • Make standard curves • Test samples • Compared values with the spec. (Hach kit) • Spiked samples to determine % recovery

  8. Major Industries That Pollute • Brunner Island • PH Glatfelter • Baker Refractories • Lehigh Portland Cement

  9. Other Pollution • Farmland • Nitrates • Urban/Storm Runoff • Industrial Waste • Municipal Waste • Source:

  10. Cleanup Acts • Codorus Creek Cleanup June 2002 • Source: www.pawatersheds.org

  11. Analysis of Chloride Testing performed by Kim and Jamie

  12. Chloride Analysis • Method from Quantitative Chemical Analysis by Daniel C. Harris • Used in Class previously • Found on page 859-860 of text • Acceptable levels of Chloride are 0.01 ppm • www.epa.gov

  13. Method • Standard Curve • 0.03 g Dextrin to 50 mL of known conc. Plus 5 drops of dichlorofluorescein • 1ppm, 0.8 ppm, 0.6 ppm, 0.2 ppm, 0.05 ppm, and 0.01 ppm of chloride • Titrated with 4 g of AgNO3 dissolved in 200 mL DI water • Titrated until pink endpoint

  14. Samples • 50 mL of sample put into Erlenmeyer Flask with 0.03 g Dextrin • Added 5 drops of dichlorofluorescein • Titrated with AgNO3 to a pink endpoint

  15. Titration and Spec. Data

  16. Spikes

  17. Results • Different levels of chloride at different points along the Codorus Creek • Highest levels 0.227 ppm • Philadelphia St. • Stagnant water • Shopping cart • Lowest levels • South Branch and East Branch above Glatfelter • 0.01 ppm---acceptable limits

  18. Results…. • Spike Recovery • Average= 96.42% • 1 ppm spikes

  19. Error • Color of endpoint • Pinks hard to determine • Dull vs. bright • Samples • Occasionally 1st sample turned right away • Other 3 trials were okay

  20. Error… • Water collection • After periods of rain • Dilution errors • Pipetting • Titration errors • Color of endpoint • Hints of green when it turned pink • When poured down the drain

  21. Sulfates Testing performed by Rob and Howie

  22. Primary Source of Sulfates

  23. Worst Case Offenders - 1999 • Brunner Island – 71,188 tons • PH Glatfelter – 6,521 tons • Baker Refractories – 3,609 tons • Lehigh Portland Cement – 1,368 tons

  24. Sulfate Wet Deposition

  25. Hazards of Sulfates In Water • Below 250 ppm no direct harm to people • Causes acidification • Kills fish • Decreases biodiversity • Causes chronic stress • At pH 5.0 most fish eggs can’t hatch

  26. Effects of pH

  27. Long-Term Trend in Stream Chemistry

  28. Sulfate Analysis: Baseline • 90 mL distilled water • 10 mL BaCl2 • Take 20 mL off top • 3 drops calmagite • Titrate with EDTA • Get Standard Zero

  29. Sampling Procedure • 90 mL Sample • 10 mL BaCl2 • Allow to precipitate overnight • Pull 20 mL off top • 3 drops calmagite • Titrate with EDTA • Average Titrations

  30. Formulas • Standard Zero – Average Titration • Divide by 1000 • Multiply by .0434 M EDTA • Multiply by mw SO4 (96) • Divide by .09 L (Amount of water sample) • Get ppm

  31. Spikes • 3 different distilled water samples (.1 L) • Added sodium sulfate (mw = 142.04 g) • #1 - .0087 g = 58.8 ppm Got 48.2 ppm • #2 - .0493 g = 333.4 ppm Got 315.7 ppm • #3 - .1194 g = 807.5 ppm Got 733.6 ppm

  32. Location Test Kit (ppm) Titration Results (ppm) Below PHG 80 26.39 / 51.0 Below Dam 37.03 Indian River 9.26 Above Spring Grove 11 6.02 Philadelphia St 10.65 Results Trial 1

  33. Location Test Kit (ppm) Titration Results (ppm) South Branch 6 18.5 Below Dam 7 6.02 Indian River 19 18.5 Above Dam 6 9.3 Results Trial 2

  34. Sources of Error • Determination of titration endpoint • Titration errors • Precipitation time • Measurements • Quantity of original sample • Testing performed by John

  35. Sulfitesin theCODORUS! KI-KIO3 volumetric method Performed by John

  36. What are sulfites used for? • Used to sanitize and preserve foods • Used in the wine industry as an antioxidant and antimicrobial • Dehydration of fruits and vegetables • Wood pulping and paper making

  37. Causes allergic reactions in asthmatics FDA and ATF have mandated that sulfites in foods at levels of 10 ppm or higher be reported on labels Effects of sulfites

  38. Procedure • Standard potassium iodide-iodate titrant(diluted 100 times from procedure found in Standard Methods for Water and Wastewater) • Starch indicator

  39. KI-KIO3 • ~.4400 g anhydrous KIO3 • 4.35 g KI • .0310 g sodium bicarbonate • Place in 1000 ml volumetric flask and fill to the mark

  40. Starch indicator • Boil 100 ml water • Weigh out 1 g of starch and place in 10 ml of water • Pour paste into boiling water • Boil until clear • Must be made before every class

  41. Put it all together! • In 250 ml flask • 1 ml sulfuric acid • .1 g sulfamic acid • 50 ml water sample • 1 ml starch indicator • Titrate with KI- KIO3 until blue

  42. Calculation of Sulfites • Used known amounts of sodium sulfite to create calibration curve • Calculated amount of sulfites from equation by plugging in the amount of titrant used

  43. Data • Minimum detectable limits 2 mg/L = 2 ppm • All data came out negative except Philadelphia street from both days and the east branch from day two • Most data below minimum detectable limits

  44. Data

  45. Day 1 Philadelphia Street .96 ppm 1.92 ppm 3.20 ppm Day 2 East Branch below .32 ppm .96 ppm Philadelphia Street .32 ppm .96 ppm East Branch above dam 2.24 ppm 1.28 ppm Results

  46. Spikes • Added a 2.508 x 10-7 M solution of sodium sulfite • About doubled the level of sulfites in the water • Made all of the samples above the detectable limit

  47. Conclusions • The levels of sulfites in the water is below detectable levels • Error • Calibration curve • Detecting endpoint

  48. Ca2+ and Mg2+ Concentrations By Jennie Waughtel And George Collins

  49. Points of Interest There are no minimum or maximum standards set by the EPA Raw Water Data from The York Water Company Ca concentration (ppm): Mg Concentration (ppm):

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