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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction

ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction. step-by-step method development. Goal of Six-Step Mode. Isolation Purification Trace enrichment. Six-Step Method Development. Compile known parameters Tech Support Form Follow step-by-step guide Fill in method development form.

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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction

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  1. ENVIRONMENTALANALYSISI. Solid Phase Extraction step-by-step method development

  2. Goal of Six-Step Mode • Isolation • Purification • Trace enrichment

  3. Six-Step Method Development • Compile known parameters • Tech Support Form • Follow step-by-step guide • Fill in method development form

  4. Technical Support Form

  5. Pertinent Data • The analyte(s) • The matrix • The analytical method • Existing method(s)

  6. The Analyte • Structure • pKa(s) • Concentration • Sample volume • Solubility • Stability

  7. The Matrix • Type of matrix • pH and ionic strength • Interferences

  8. The Analytical Method • Final technique • Compatible solvents • HPLC conditions

  9. Existing Method • Liquid-liquid method • Current SPE method details • Data from current method

  10. Dr. Anna Light Pollution Unlimited 1224 Sunnyside Drive Elution, Alaska (907) 663-3217 573 (907) 663-3218 Method Development Example

  11. The Analyte

  12. The Analyte (cont.)

  13. The Matrix

  14. The Analytical Method

  15. Other Information

  16. Following the Guide

  17. The “Form” Sample name _________________ Analyte of Interest ________________ Sample size ____________________ Sorbent Bed Mass _______ Cartridge volume_____ Sorbent phases to try 1) _____ 2) _____ 3) _____ 4) _____ 1. Sample pretreatment ___________________________ 2. Condition column with ____ mL of _________ at ___ mL/min 3. Equilibrate column with ____ mL of _________ at ___ mL/min. 4. Load sample at ______ mL per minute. 5. Remove interference with ____ mL of _________ at ___ L/min. Drying step _____ minutes 6. Elute analyte with ____ mL of _________ at ___ mL/min. Remember to include soak step if possible!

  18. Filling in the Form

  19. Following the Guide

  20. Sample Size Determination

  21. Filling in the Form

  22. Sorbent Capacity Hydrophobic phases: 1- 5% of Sorbent Mass Ion Exchangers 0.3 to 0.6 milli-equivalents per gram

  23. Following the Guide

  24. Select a Mechanism

  25. Select a Mechanism

  26. Select a Mechanism

  27. Select a Mechanism

  28. Following the Guide

  29. Selecting a Sorbent

  30. Filling in the Form

  31. Following the Guide

  32. A Reminder...

  33. Sample Pretreatment

  34. Filling in the Form

  35. Following the Guide

  36. Conditioning and Equilibration

  37. Conditioning and Equilibration

  38. Filling in the Form

  39. Following the Guide

  40. Sample Loading Rate

  41. Filling in the Form

  42. Following the Guide

  43. Removing Interferences

  44. Removing Interferences

  45. Filling in the Form

  46. Following the Guide

  47. Drying Time

  48. Filling in the Form

  49. Following the Guide

  50. Selecting an Elution Solvent

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