1. PS 26 Playground - Soil Analysis Analytical Chemistry of Pollutants Dr. Joe Gardella Todd M. Alonzo, Dominic O. Hull, Doris J. Glykys, Ed Tasber, and David G. Twoey

2. Why Did We Choose PS26? b Soil Analysis b GC/MS b Elemental Analysis - Why Lead? Requested by CommunityRequested by Community Buffalo ChinaBuffalo China Very Toxic MetalVery Toxic Metal

3. Sampling Technique b Donned Gloves and Safety Glasses b Spade Rinsed with 50/50 v/v Nitric Acid/DI Water b Dig Hole and Obtain sample at 6” Depth b Refill Hole b Jars Amber to Avoid Photolysis No Head Space Above Sample Sealed with Foil Cooled on Dry Ice

4. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

5. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

6. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

7. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

8. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

9. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

10. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

11. Sampling Sites       Synthetic Organic Compounds  Lead Harrison St. (Dead End) 

12. Elemental Analysis b Digestion b Flame Atomic Absorption Spectroscopy b Inductively Coupled Plasma / Atomic Emission Spectroscopy b Standard Addition b Results

13. Digestion b EPA Method 3050 Successive Nitric Acid Additions and RefluxSuccessive Nitric Acid Additions and Reflux Reduce VolumeReduce Volume Peroxide NeutralizationPeroxide Neutralization Reduce VolumeReduce Volume –GFAA and ICP/MS Addition of HCl AcidAddition of HCl Acid –FLAA and ICP/AES

14. Direct Aspiration Atomic Absorption Spectroscopy (FLAA) b A sample is aspirated and atomized in a flame. b A characteristic light beam is directed through the flame into a monochromator, and onto a detector that measures the amount of absorbed light. b Absorption depends upon the presence of free unexcited ground-state atoms in the flame. »Beer-Lambert Law

15. Standard Addition b The preparation of standards that match the samples is often impossible or extremely difficult. b The preparation of standards that match the samples is often impossible or extremely difficult. b Accurate determinations are possible by making the concentration calibration in the presence of the matrix. b By adding aliquots of a standard to portions of the sample, any interferent present in the sample will affect the standard and sample absorbance similarly.

16. If Interferences are present: b The number of ground state atoms producing atomic absorption will be affected. b The absorbance increase from the added standard will also change by the same proportional amount since the concentration of interferent is the same in each solution.

17. Determination of Concentration

18. Comparison of Lead Results

19. Synthetic Organic Analysis b Digestion b Volume Reduction b GC-MS Analysis b Qualitative Analysis b Quantitative Analysis

20. Digestion b EPA Method 3550 –Addition of NaSO 4 –Successive Addition of 50/50 v/v Methylene Chloride/Acetone with Ultrasonic Extraction –Vacuum Filtration –Reduce Volume

21. GC-MS Analysis b Separation of Components –Using Capillary Column –by Molecular Weight b Mass Analysis –Fragmentation of Compounds –Mass Separation by Mass-Charge Ratio

22. Qualitative Results b Acenaphthene b Anthracene b Bis(2-ethylhexyl) Phthalate b Dibenzofuran b Fluranthene b Fluorene b 2-Methyl- Naphthalene b Naphthalene b Pyrene b 4-Fluoro-1,1’-Biphenyl b 1,2-Dihydro- Acenaphthylene

23. Quantitative Analysis

24. Conclusions b Lead and PAHs were detected in the soil b Concentration of lead in the park was below action level b Concentration of lead at the dead end was above 400 ppm level b Many of the PAHs detected could not be quantified