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Published byCleopatra Lynne Underwood Modified over 9 years ago
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ENVIRONMENTAL ANALYSIS I. Solid Phase Extraction introduction sample preparation overview
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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
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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
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ApplicationsApplications v EPA 1664: O & G v EPA 525.1 Analytes v Extraction of Triazines v Extraction of PAHs v Multiresidue Method for Pesticides
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Sample Preparation Overview
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Sample Preparation v THE GOAL ä Prepare sample for a particular analytical technique ä Interference removal ä Concentration v THE BASIS ä Phase transfer
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Phase Choices Liquid VaporDistillation Soln. SolidPrecipitation Soln. Soln.L/L extraction Soln. SurfaceLiquid sorption Vapor SurfaceGas sorption Solid Soln.Soxhlet Solid FluidSFE
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Phase Transfer Efficiency
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V ORG V AQ V ORG V AQ 1 1 K ( ) + 1 % E = 100 x n n Phase Ratio: = (V ORG / V AQ )
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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
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Continuous L/L Extraction Likens-Nickerson apparatus
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Continuous L/L Extraction Nielsen-Kryger apparatus
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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
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Interference Removal(1) before.. after DIOL SPE
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Interference Removal(2a) 10g sample after ENV+ extraction
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Interference Removal(2b) ENV+ extract after PRS clean-up
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