Steam distillation is a special type of distillation for temperature sensitive materials like natural aromatic compounds. When two immiscible liquids are distilled, the total vapor pressure above the liquid is equal to the sum of the vapor pressure of each compound. Steam distillation allows distillation of organic compounds with high boiling points to distill below 100 oC avoiding decomposition.
Steam distillation is a special type of distillation for temperature sensitive materials like natural aromatic compounds. When two immiscible liquids are distilled, the total vapor pressure above the liquid is equal to the sum of the vapor pressure of each compound. Steam distillation allows distillation of organic compounds with high boiling points to distill below 100 oC avoiding decomposition.
Steam distillation is a special type of distillation for temperature sensitive materials like natural aromatic compounds. When two immiscible liquids are distilled, the total vapor pressure above the liquid is equal to the sum of the vapor pressure of each compound. Steam distillation allows distillation of organic compounds with high boiling points to distill below 100 oC avoiding decomposition.
Steam Distillation Definition Steam Distillation is a special type of distillation for temperature sensitive materials like natural aromatic compounds. -This distillation can be performed on two immiscible liquids so called codistillation. - When two immiscible liquids are distilled, the total vapor pressure P T above the liquid is equal to the sum of the vapor pressure of each compound. This relationship is known as Daltons Law. - P T is not dependent on mole fraction of each component which would be included if the liquids were miscible, because the vaporization of each liquid is independent of the other. - Advantage : steam distillation allows distillation of organic compounds with high boiling points to distill below 100 C avoiding decomposition. Essential Oils A volatile oil, usually having the characteristic odor or flavor of the plant, frequently is a water-immiscible liquid separated by distillation from the plant material. Such oils are used to make perfumes, flavorings, cosmetics, incenses, and medicine. For example: Clove oil consists of several compounds such as eugenol, which is the major component (85-90%) and eugenol acetate (9-10%). Eugenol has a boiling temperature of 254 C. Steam Distillation Set Up claisen adapter rubber bands stopper instead of thermometer 125 mL erlenmeyer flask fill with H 2 O mark level with marker 500 mL flask with boiling chip Changes from the Lab Manual 1. Use 10 grams of powdered cloves rather than 5 grams of whole cloves. 2. Use 500 mL round bottom flask rather than a 100 mL round bottom flask. 3. Collect distillate in a 125 mL Erlenmeyer flask. 4. Use a hot plate for your heat source rather than a heating mantle. 5. Use ether to extract the distillate rather than methylene chloride. Formation of big bubbles during the distillation Adding Cloves into the round bottom flask using the stemless funnel Clove Powder in the Flask Experimental Procedure Steam Distillation: Don't forget to apply grease at every glass joint. Distill at a steady rate (try distilling at 1 drop per 2 seconds). Maintain water level by adding water from the addition funnel. Distill until no oily layer is apparent. Collect at least 100 mL of distillate. Extraction: Transfer distillate to a separatory (sep) funnel and add 10 mL of saturated NaCl solution to the sep funnel. Rinse condenser and receiving flask each with 5 mL of ether and transfer this to the separatory funnel. Swirl gently and vent the sep funnel. THEN vigorously shake with frequent venting.
ether layer aqueous layer - Drain the aqueous layer. Transfer the ether layer (top layer) to a 50 mL flask and return the aqueous layer (bottom layer) to the sep funnel. - Rinse two more times with 5 mL portions of ether. With each step combine the ether layers and repeat extraction of the aqueous layer with the combined ether layers. - Dry the combined ether extracts over anhydrous Na 2 SO 4 for 5 minutes. Decant as much as possible before removing balance with pipet. - Filter ether solution through a cotton plugged pipet into a preweighed 50 mL round bottom flask - Rinse the Na 2 SO 4 with three additional 2-mL portions of ether and filter into the preweighed 50 mL round bottom flask. Simple Distillation: - Remove ether by simple distillation. Place your receiver in an ice bath. - Then remove last traces of ether with House Vacuum. Simple Distillation remove claisen adapter rubber bands stopper instead of thermometer round bottomed collection flask in an ice bath 50 mL flask with boiling chip remove addition funnel - Determine % recovery of eugenol. DO NOT dissolve eugenol in methanol!!!! Waste: - 1 bottle is in the hood for ether / water waste. - DO NOT collect cloves! Decant water into sink, put cloves in a paper towl and throw away in trash can. - Next week, converting eugenol to the ester derivative Omit : 1. TLC 2. The qualitative tests described in the module. Don't forget: You will also weigh, perform TLC, and measure the melting point for each of your compounds from last week. You need to submit your samples in marked vials as instructed by your TA. You must turn in your TLC plates with your lab report in an envelope. Final Notes