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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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environmental analysis i solid phase extraction

ENVIRONMENTALANALYSISI. Solid Phase Extraction

introduction

sample preparation overview

basic principles of spe
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
recent developments in spe
Recent Developments in SPE
  • Resin-Based Sorbents
  • Carbon-Based Sorbents
  • ISOLUTE HM-N Sorbent
  • Phase Separators
  • MSPD: Matrix Solid Phase Dispersion
  • Dispersive SPE
applications
Applications
  • EPA 1664: O & G
  • EPA 525.1 Analytes
  • Extraction of Triazines
  • Extraction of PAHs
  • Multiresidue Method for Pesticides
sample preparation
Sample Preparation
  • THE GOAL
    • Prepare sample for a particular analytical technique
    • Interference removal
    • Concentration
  • THE BASIS
    • Phase transfer
phase choices
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

phase transfer efficiency9

1

K( ) + 1

VORG

VAQ

Phase Transfer Efficiency

n

% E = 100 x

  • Phase Ratio: b = (VORG / VAQ)
l l extraction
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
continuous l l extraction
Continuous L/L Extraction

Likens-Nickerson apparatus

continuous l l extraction12
Continuous L/L Extraction

Nielsen-Kryger apparatus

solid phase extraction
Solid 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)

before..

after

DIOL SPE

interference removal 2a
Interference Removal(2a)

10g sample

after ENV+

extraction

interference removal 2b
Interference Removal(2b)

ENV+ extract

after PRS

clean-up