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sample preparation
techniques for water
analysis.
Dr S. D. M. Chinthaka
Department of Chemistry
University of Sri Jayewardenepura
Liquid-Liquid Extraction
❑ Historically the first sample preparation technique used in
analytical chemistry.
½ Cu2+
H+
Liquid-Liquid Extraction
Liquid –liquid extraction of metal ions
Liquid-Liquid Extraction
Factors affecting the stability the metal ion complexes
pH1/2
p
H
Liquid-Liquid Extraction
E vs pH
Liquid-Liquid Extraction
Problems with Liquid –liquid extraction
❑ Emulsion formation
❑ Time consuming
❑ Difficult automation
❑ Less green
Liquid-Liquid Extraction
Solutions for the drawbacks of Liquid –liquid extraction
Micro –liquid-liquid
extraction
Diethyl ether
[AA] (non polar)
❖ Highly selective
Applications of HPLLME
Head phase
Liquid-Liquid Extraction
Direct immersion
Liquid-Liquid Extraction
Advantages
❖ Simplicity
❖ Ease of implementation
Advantages/disadvantages of HS-
SDME
❖ Rapid stirring is not possible
❖ Good for volatile and semi-volatile analytes
❖ low non-volatile matrix interferences
❖ Aqueous phase mass transfer step is critical
low vapor pressure solvents must be selected
Liquid-Liquid Extraction
Dynamic liquid/liquid microextraction
(SDME)
Liquid-Liquid Extraction
Continuous flow Single drop liquid/liquid microextraction (SDME)
Liquid-Liquid Extraction
❑ The above the CMC and above the cloud point temperature,
the surfactant forms surfactant rich phase(micells) and
surfactant poor phase.
Surfactant poor
phase
Surfactant rich
phase
1
Solvent free Extractions
❑ Polarity of analyte
❑ Dehydration
❑ Extraction
Advantages:
❑ Isolation and clean - up in one step