ENVIRONMENTALENVIRONMENTALANALYSISANALYSISI. Solid Phase ExtractionI. Solid Phase Extraction

ENVIRONMENTALENVIRONMENTALANALYSISANALYSISI. Solid Phase ExtractionI. Solid Phase Extraction

introduction

sample preparation overview

Basic Principles of SPEBasic Principles of SPEBasic Principles of SPEBasic 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

Recent Developments in SPERecent Developments in SPERecent Developments in SPERecent Developments in SPE

Resin-Based Sorbents

Carbon-Based Sorbents

ISOLUTE HM-N Sorbent

Phase Separators

MSPD: Matrix Solid Phase Dispersion

Dispersive SPE

ApplicationsApplicationsApplicationsApplications

EPA 1664: O & G

EPA 525.1 Analytes

Extraction of Triazines

Extraction of PAHs

Multiresidue Method for Pesticides

Sample Sample Preparation Preparation OverviewOverview

Sample Sample Preparation Preparation OverviewOverview

Sample PreparationSample PreparationSample PreparationSample Preparation

THE GOAL Prepare sample for a particular

analytical technique Interference removal Concentration

THE BASIS Phase transfer

Phase ChoicesPhase ChoicesPhase ChoicesPhase 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

PhasePhaseTransferTransferEfficiencyEfficiency

PhasePhaseTransferTransferEfficiencyEfficiency

Phase Transfer EfficiencyPhase Transfer EfficiencyPhase Transfer EfficiencyPhase Transfer Efficiency

VORG

VAQ

VORG

VAQ

11

K ( ) + 1K ( ) + 1% E = 100 x% E = 100 x

nn

Phase Ratio: = (VORG / VAQ)Phase Ratio: = (VORG / VAQ)

L / L ExtractionL / L ExtractionL / L ExtractionL / 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

Continuous Continuous L/L ExtractionL/L ExtractionContinuous Continuous L/L ExtractionL/L Extraction

Likens-Nickerson apparatus

Continuous Continuous L/L ExtractionL/L ExtractionContinuous Continuous L/L ExtractionL/L Extraction

Nielsen-Kryger apparatus

Solid Phase ExtractionSolid Phase ExtractionSolid Phase ExtractionSolid Phase Extraction

Sorbent-phase and Liquid-phase Inherent immiscibility Selective extraction No emulsions Small solvent volumes Inherent concentration Batch process

Interference Removal(1)Interference Removal(1)Interference Removal(1)Interference Removal(1)

before..

afterDIOL SPE

Interference Removal(2a)Interference Removal(2a)Interference Removal(2a)Interference Removal(2a)

10g sample after ENV+ extraction

Interference Removal(2b)Interference Removal(2b)Interference Removal(2b)Interference Removal(2b)

ENV+ extractafter PRSclean-up