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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction

ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction. introduction sample preparation overview. Basic Principles of SPE. Sample Preparation Overview Fundamentals of SPE Sorbent Selection in SPE Various Modes of SPE Packed Bed vs. Disk vs. Tip Format The use of Dual Phases

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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction

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  1. ENVIRONMENTALANALYSISI. Solid Phase Extraction introduction sample preparation overview

  2. Basic Principles of SPE • Sample Preparation Overview • Fundamentals of SPE • Sorbent Selection in SPE • Various Modes of SPE • Packed Bed vs. Disk vs. Tip Format • The use of Dual Phases • Step by Step Method Development

  3. Recent Developments in SPE • Resin-Based Sorbents • Carbon-Based Sorbents • ISOLUTE HM-N Sorbent • Phase Separators • MSPD: Matrix Solid Phase Dispersion • Dispersive SPE

  4. Applications • EPA 1664: O & G • EPA 525.1 Analytes • Extraction of Triazines • Extraction of PAHs • Multiresidue Method for Pesticides

  5. Sample Preparation Overview

  6. Sample Preparation • THE GOAL • Prepare sample for a particular analytical technique • Interference removal • Concentration • THE BASIS • Phase transfer

  7. Phase Choices Liquid  Vapor Distillation Soln.  Solid Precipitation Soln.  Soln. L/L extraction Soln.  Surface Liquid sorption Vapor  Surface Gas sorption Solid  Soln. Soxhlet Solid  Fluid SFE

  8. PhaseTransferEfficiency

  9. 1 K( ) + 1 VORG VAQ Phase Transfer Efficiency n % E = 100 x • Phase Ratio: b = (VORG / VAQ)

  10. L / L Extraction • Two extraction solvents per step • Solvents must be immiscible • Non-selective extraction • Emulsion • Large solvent volumes • Extract concentration required • Serial process; largely manual

  11. Continuous L/L Extraction Likens-Nickerson apparatus

  12. Continuous L/L Extraction Nielsen-Kryger apparatus

  13. Solid Phase Extraction • Sorbent-phase and Liquid-phase • Inherent immiscibility • Selective extraction • No emulsions • Small solvent volumes • Inherent concentration • Batch process

  14. Interference Removal(1) before.. after DIOL SPE

  15. Interference Removal(2a) 10g sample after ENV+ extraction

  16. Interference Removal(2b) ENV+ extract after PRS clean-up

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