Andre Hauser - kisr


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Andre Hauser - kisr

  1. 1. Near-Infrared (NIR) Spectroscopy as a Rapid Monitoring Tool for Total Petroleum Hydrocarbon (TPH) as Environmental Hazard in Contaminated Soils and Sediments<br />by<br />Andre’ Hauser*, Fatima Ali and Bashayer Al-Dosari<br />Central Analytical Laboratory, Kuwait Institute for Scientific Research, <br />P.O. Box 24885, 13109 Safat, KUWAIT<br />*<br />Tel.: 00965-4989053<br />E-Mail:<br />
  2. 2. OUTLINE<br />1. TPHs-A Short Description<br />2. Oil Pollution-A Daily Hazard<br />3. Remediation of Contaminated Areas- A Challenge<br />4. TPH Analysis- Conventional & NIR Technique<br />5. Case Study- Testing of Real Field Samples<br />6. Conventional vs. NIR Analysis- Cost, Efficiency & Throughput Considerations<br />7. Summary<br />
  3. 3. TPHsA Short Description<br />Crude Oil<br />Grease,<br />Lubricants<br />TPHs<br />(Total Petroleum Hydrocarbons)<br />TPHs<br />Refinery Products<br />Transposition Fuel<br />Weathered Oil<br />
  4. 4. TPHsA Short Description<br /><ul><li> TPHs is a classes of compounds that does not naturally</li></ul> occur in the environment<br /><ul><li>TPHs consisting mainly of C and H and to a</li></ul> much lesser extend of S, N, O and heavy metals (V, Ni)<br />
  5. 5. TPHsA Short Description<br /><ul><li> Typical entities are: Saturates,</li></ul>and heterocyclic compounds<br />aromatics<br />
  6. 6. TPHsA Short Description<br /><ul><li> Examples of TPHs</li></li></ul><li>TPHsA Short Description<br /><ul><li> TPHs differ in their toxicity
  7. 7. The higher the content of polyaromatic hydro-</li></ul> carbons (PAHs) and polar compounds (S,N,O) in<br /> TPHs the higher is their water solubility<br />WHO-Guidelines for Drinking Water<br />
  8. 8. TPHsA Short Description<br /><ul><li> In arid, oil rich countries like Kuwait high risk of</li></ul> taking up air-borne particles covered with TPHs <br /><ul><li> Some PAHs are extremely carcinogenic</li></li></ul><li>TPHsA Short Description<br />Source: CA EPA, 1999<br />
  9. 9. Oil (TPH) PollutionA Daily Hazard<br /><ul><li> Environmental disasters such as:</li></li></ul><li>Oil (TPH) PollutionA Daily Hazard<br /><ul><li> Environmental pollution by oil industry:</li></li></ul><li>Oil (TPH) PollutionA Daily Hazard<br /><ul><li> Environmental pollution by negligence:</li></li></ul><li>Remediation of Contaminated Soil A Challenging Task<br /><ul><li> Waste disposal (excavation & transportation)
  10. 10. Extraction with organic solvents (excavation &</li></ul> washing)<br /><ul><li> Bio-remediation (excavation & mixing with</li></ul> bacteria)<br /><ul><li> Agro-remediation (in situ treatment)</li></li></ul><li>Remediation of Contaminated SoilTasks for Analytical Chemistry<br /><ul><li> Screening of large areas for TPH-contamination
  11. 11. Assessment of the extent of TPH-contamination
  12. 12. Monitoring of clean up process
  13. 13. Determination of end point of clean up process</li></li></ul><li>Remediation of Contaminated Soil A Challenge for Analytical Chemistry<br /><ul><li> High number of samples
  14. 14. High throughput required
  15. 15. No or low waste disposal per sample
  16. 16. Accuracy as good as needed
  17. 17. Low cost per sample</li></li></ul><li>TPH AnalysisConventional Method vs. NIR Spectroscopy<br />
  18. 18. TPH AnalysisConventional Method<br />
  19. 19. TPH AnalysisConventional Method<br />Sample<br />Solvent<br />
  20. 20. TPH AnalysisConventional Method<br />Sample +<br />Solvent +<br />Silica Gel<br />
  21. 21. TPH AnalysisConventional Method<br />
  22. 22. TPH AnalysisConventional Method<br /><ul><li> Calibration
  23. 23. IR-Measurement</li></li></ul><li>TPH AnalysisNIR Spectroscopy<br /><ul><li>NIR is a spectroscopic technique that uses infrared (IR) light diffuse scattered on the sample surface (DRIFT) to quantify the analyte (TPHs) in a matrix (soil).</li></ul>Light Source<br />Detector<br />
  24. 24. <ul><li>While the IR-light interacts with the sample it leaves its fingerprint on the detected light</li></ul>TPH AnalysisNIR Spectroscopy<br />Light Source<br />Sample<br />Detector<br />
  25. 25. TPH AnalysisNIR Spectroscopy<br /><ul><li>NIR measures the amount of light absorbed by a sample vs. the wavelength of the IR-light. </li></ul>TPH-Signals<br />
  26. 26. TPH AnalysisNIR Spectroscopy<br /><ul><li>NIR-Spectroscopy is
  27. 27. Non-destructive</li></ul>Sample<br /><ul><li>Without sample preparation
  28. 28. No waste
  29. 29. Uses DRIFT-technique
  30. 30. Needs calibration</li></ul>NIR-spectrometer MPATM<br />from BRUKER<br />
  31. 31. TPH AnalysisNIR Spectroscopy<br /><ul><li>Calibration
  32. 32. NIR predicts TPH-concentration using spectra from </li></ul> similar samples (Reference Value) with known TPH-<br />concentration<br /><ul><li>NIR uses calibration equations (Model)
  33. 33. Calibration equations are found by chemometric</li></ul> methods such as principal component analysis (PCA) and principal component regression (PCR) <br /><ul><li> Result: Model (equation) were TPH-</li></ul> concentration is correlated with NIR-spectral <br /> features (wavelength, intensity, spectral shape)<br /><ul><li> QC of the model by cross-validation:</li></ul> Correlation coefficient (R2)≈ 1<br /> Root mean square error (RMSE) ≈ 0.1<br />
  34. 34. TPH AnalysisNIR Spectroscopy<br /><ul><li>Reference samples (S =43)</li></li></ul><li>TPH AnalysisNIR Spectroscopy<br /><ul><li>Cross validation of the model (PCA-Equation)</li></ul> Cross validation result: R2 = 0.9415; RMSE = 0.158<br />
  35. 35. Case StudyTesting of Real Field Samples<br /><ul><li>Field samples (S =24)</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Field samples were analyzed by conventional (certified) and NIR technique
  36. 36. Data from conventional technique were considered as true
  37. 37. Comparison between data from both technique</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Comparison of data from all field samples</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Comparison of data from Kuwait Soil (north) samples</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Comparison of data from Kuwait Soil (north) samples contaminated by weathered oil</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Comparison of data from sediment samples contaminated by atmospheric residue</li></li></ul><li>Case StudyTesting of Real Field Samples<br /><ul><li>Comparison of data from certified soil samples contaminated by atmospheric residue</li></li></ul><li>Conventional vs. NIR AnalysisCost, Efficiency & Throughput Considerations<br />
  38. 38. Summary<br /><ul><li>Total petroleum hydrocarbons (TPHs) are a mix of petroleum based chemicals that do not exist naturally in the environment
  39. 39. TPHs in the environmentpose a potential health risk to humans and destroy the nature
  40. 40. TPH-contaminated areas need to be identified, their health risk assessed and cleaned up
  41. 41. TPH-quantification is inevitable for hazard evaluation and clean-up activities
  42. 42. Conventional technique for TPH-quantification are regulated by EPA & ASTM
  43. 43. Conventional technique is time consuming, costly and harmful to the environment
  44. 44. Near infrared (NIR) spectroscopycan replace conventional technique </li></li></ul><li>Summary<br /><ul><li>Advantages of NIR: Environmentally friendly, fast and cost effective
  45. 45. Disadvantages of NIR: Large-scale calibration needed, high detection limit (%) and medium accuracy
  46. 46. NIR is the method of choice for monitoring soil clean-up:
  47. 47. TPHs in %-range
  48. 48. Large number of samples
  49. 49. Trend monitoring
  50. 50. End point determination</li></li></ul><li>Thank You!<br />Q & A<br />
  51. 51. Contacts<br />Research Specialist: Dr. Andre’ Hauser <br /><ul><li>Tel.: 24989053;</li></ul>Research Specialist/Section Head: Dr. Fatima Ali <br /><ul><li>Tel.: 24989050; e-Mail:</li></ul>Technician Ms. Bashayer Al-Dosery<br />