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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction introduction sample preparation overview.

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Presentation on theme: "ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction introduction sample preparation overview."— Presentation transcript:

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2 ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction introduction sample preparation overview

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

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

5 ApplicationsApplications v EPA 1664: O & G v EPA 525.1 Analytes v Extraction of Triazines v Extraction of PAHs v Multiresidue Method for Pesticides

6 Sample Preparation Overview

7 Sample Preparation v THE GOAL ä Prepare sample for a particular analytical technique ä Interference removal ä Concentration v THE BASIS ä Phase transfer

8 Phase Choices Liquid  VaporDistillation Soln.  SolidPrecipitation Soln.  Soln.L/L extraction Soln.  SurfaceLiquid sorption Vapor  SurfaceGas sorption Solid  Soln.Soxhlet Solid  FluidSFE

9 Phase Transfer Efficiency

10 V ORG V AQ V ORG V AQ 1 1 K ( ) + 1 % E = 100 x n n Phase Ratio:  = (V ORG / V AQ )

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

12 Continuous L/L Extraction Likens-Nickerson apparatus

13 Continuous L/L Extraction Nielsen-Kryger apparatus

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

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

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

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


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