environmental analysis i. solid phase extraction introduction sample preparation overview
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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
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
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