ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction introduction sample preparation overview

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

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

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

Sample Preparation Overview

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

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

Phase Transfer Efficiency

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

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

Continuous L/L Extraction Likens-Nickerson apparatus

Continuous L/L Extraction Nielsen-Kryger apparatus

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

Interference Removal(1) before.. after DIOL SPE

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

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