======Using a Separating Funnel====== **Materials: **{{$demo.materials_description}}\\ **Difficulty: **{{$demo.difficulty_description}}\\ **Safety: **{{$demo.safety_description}}\\ \\ **Categories:** {{$demo.categories}} \\ **Alternative titles:** Liquid–Liquid Extraction ====Summary==== {{$demo.summary}} ====Procedure==== - Clamp the separatory funnel securely by the neck; ensure the stopcock is closed and place a labeled receiving flask beneath the stem. - Add the first liquid phase to the funnel, then add the second immiscible phase (commonly, organic solvent and water). Insert the stopper firmly. - Support the stopper with one hand and the stopcock with the other; invert the funnel and gently swirl to mix. - Vent immediately by opening the stopcock while the funnel is inverted and pointed away from people and equipment; close and repeat a mix–vent cycle several times. - Return the funnel to the ring stand and allow the layers to separate fully (wait until a sharp interface forms). - Identify which layer is which: compare known densities, or add a drop of water—if the drop joins the lower layer, the lower layer is aqueous. - Drain the bottom layer slowly into a labeled flask, stopping just before the interface reaches the stopcock. - Remove the funnel from the clamp and pour the top layer out of the top into a second labeled flask to avoid contaminating it with residual bottom-layer hold-up in the stopcock channel. - For improved recovery, perform multiple small-volume extractions rather than a single large one; combine like layers as appropriate. - Dry the organic layer if needed by adding a suitable anhydrous drying agent (e.g., magnesium sulfate or calcium chloride), swirl, wait a few minutes, and decant or filter off the dry solution. ====Links==== Using a Separating Funnel - Cormac Quigley: {{youtube>L13QUwqKwlU?}}\\ How to Use a Separatory Funnel - Chemistry in a Nutshell: {{youtube>6iB2U0RZLjc?}}\\ ====Variations==== * Demonstrate an extraction with colored solutes (e.g., iodine in an organic solvent, then extract into aqueous iodide) to visualize partitioning. * Show “salting out” by adding sodium chloride to the aqueous phase to reduce emulsion formation and shift distribution. * Run a microscale version in a centrifuge tube with a Pasteur pipette as a mini-separator for rapid trials. * Quantify extraction efficiency by measuring color intensity or absorbance of each layer and comparing single vs. multiple extractions. ====Safety Precautions==== * Wear splash goggles, lab coat, and appropriate chemical-resistant gloves; conduct work in a fume hood when using volatile or hazardous solvents. * Always vent the funnel away from people—pressure can build rapidly with volatile solvents or acid/base reactions. * Keep a firm grip on the stopper and stopcock while shaking; do not clamp the funnel while shaking. * Check that the stopcock is closed before filling and that all joints are secure to prevent spills. * Dispose of waste properly (e.g., segregate halogenated and non-halogenated organic waste; never pour organic solvents down the drain). ====Questions to Consider==== * Why is venting necessary during shaking? (Mixing can generate vapor pressure or gases; venting prevents dangerous pressure buildup.) * How can you confirm which layer is the aqueous layer? (Compare densities or add a drop of water to see which layer it joins.) * Why are several small extractions more effective than one large extraction with the same total volume? (Partitioning is governed by the distribution coefficient; multiple contacts extract a greater fraction overall.) * What causes emulsions and how can you break them? (Fine dispersions form from vigorous mixing or surfactants; allow time, add salt, gently swirl, or use a small amount of a mutually soluble solvent.) * Why dry the organic layer before evaporation? (Dissolved water carries impurities and can reduce yield or purity; drying agents remove residual moisture.)