Solvent Extraction by Flow Injection Method
1. Introduction
Solvent extraction, also known as liquid–liquid extraction (LLE), is a widely used separation
technique that involves the transfer of a solute from one liquid phase (usually aqueous) to
another immiscible liquid phase (usually organic). This method is commonly used in
analytical chemistry, hydrometallurgy, pharmaceuticals, and environmental studies.
When solvent extraction is coupled with Flow Injection Analysis (FIA), the process becomes
faster, automated, and more reproducible. This combination allows for rapid quantitative
determinations with minimal manual handling and reagent consumption.
2. Principle of Solvent Extraction in FIA
The basic principle involves the partitioning of an analyte between two immiscible liquid
phases—an aqueous phase and an organic solvent phase—based on their solubility
differences.
In Flow Injection Analysis, a small, known volume of the sample solution is injected into a
continuously flowing carrier stream. As the sample moves through the system, it merges
with the organic solvent stream containing the extractant. Mixing occurs in a reactor coil,
allowing the analyte to transfer from one phase to another.
After extraction, the two phases are separated using a phase separator, and the phase
containing the analyte (usually the organic one) is directed toward a detector for
measurement, often a spectrophotometer.
The efficiency of extraction depends on:
• The distribution coefficient (KD) of the analyte
• The pH of the aqueous phase
• The nature of the extractant and solvent
• The contact time between the two phases
3. Instrumentation Setup
A typical solvent extraction FIA system consists of the following components:
1. Carrier stream – Generally an aqueous solution that transports the sample through the
system.
2. Sample injector – Introduces a fixed volume of the sample into the carrier stream.
3. Mixing coil / reactor – Ensures proper mixing between the aqueous and organic phases to
allow analyte transfer.
4. Phase separator – Separates the two immiscible liquids (organic and aqueous).
Hydrophobic membranes or gravity-based separators are commonly used.
5. Detector – Measures the analyte concentration in the extracted phase (e.g., UV-Visible
spectrophotometer, fluorimeter).
6. Pump system – Controls and maintains constant flow rates for carrier and reagent
streams.
4. Experimental Procedure
1. The aqueous sample solution is injected into a carrier stream flowing through the system.
2. This stream meets the organic solvent stream containing the extractant.
3. The two immiscible streams are thoroughly mixed in a reaction coil, allowing the analyte
to move from the aqueous phase to the organic phase.
4. The mixture enters the phase separator, where the phases are separated.
5. The organic phase (containing the analyte) is directed to a detector.
6. The signal generated is recorded and is proportional to the analyte concentration.
5. Advantages of Solvent Extraction FIA
• Automation: Minimizes manual operations and human error.
• Speed: Rapid analysis (seconds to minutes per sample).
• High precision and reproducibility: Controlled flow conditions ensure consistent results.
• Low reagent and sample consumption: Environmentally friendly and cost-effective.
• Ease of coupling: Can be linked to various detectors (UV–Vis, AAS, fluorimetric).
• Continuous operation: Ideal for online or real-time process monitoring.
6. Applications
Solvent extraction FIA has a wide range of applications in different fields:
• Environmental analysis: Determination of trace metals in water samples (Fe³⁺, Cu²⁺, Co²⁺,
Ni²⁺, Pb²⁺).
• Pharmaceutical industry: Analysis of active ingredients and purity testing.
• Industrial process monitoring: Used in hydrometallurgy and process control for metal
recovery.
• Food and agricultural analysis: Determination of trace nutrients or contaminants.
7. Example: Determination of Iron (III)
Objective: To determine Fe³⁺ concentration using solvent extraction FIA.
Procedure:
1. Fe³⁺ ions in aqueous phase react with 8-hydroxyquinoline (oxine) to form a yellow
complex.
2. The complex is extracted into chloroform (organic phase).
3. The organic layer is separated and passed through a UV–Visible detector.
4. The absorbance is measured at ~410 nm.
5. A calibration curve is used to determine the Fe³⁺ concentration in unknown samples.
This method provides rapid, reproducible, and accurate results compared to conventional
batch extraction methods.
8. Limitations
• Requires precise control of flow rate and mixing conditions.
• Limited to analytes that can effectively partition between two phases.
• The phase separator can be sensitive to pressure or flow fluctuations.
• Not suitable for very viscous or emulsifying sample matrices.
