Experiment 7- Isolation of the Major Component of Clove Oil
Pre-Lab Questions: 1.) Briefly explain the concept of steam distillation. What is the difference between a simple distillation and a steam distillation? When a mixture of two immiscible liquids are distilled it is referred to as codistillation. This process is referred to as steam distillation when one of the liquids is water. This distillation is used to separate organic liquids from natural products and reaction mixtures in which the final product results in high boiling residues such as tars, inorganic salts, and other relatively involatile components. It is useful in isolating volatile oils from various parts of plants and not useful in the final purification of a
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Weigh them in a tared weighing dish. My partner ground the cloves the amount of cloves we had was 5.03 grams. 2.) Assemble an apparatus for steam distillation using a large (250-500ml) boiling flask and a steam trap, and have your instructor check your apparatus. Apparatus was successfully assembled. 3.) Combine the ground cloves with 50ml of water in the boiling flask then; steam distill the mixture to obtain the clove oil. Continue the distillation until a drop or two of the emerging distillate, collected on a watch glass, is odorless and water-clear; with no oily droplets. 150ml might need to be distilled before it becomes clear. Vent the steam line or raise the steam inlet tube above the liquid level in the boiling flask before you turn off the steam. Took about 20-30 minutes for emerging distillate to drop on watchglass and first few drops seemed clear. But we went ahead and placed a flask and started collected liquid because the process of distilling 150ml of fluid was taking quite some time. A sufficient amount of fluid was collected and checked by Professor.
Extraction of Clove Oil After Distillation 1.) Transfer the distillate to separatory funnel. Fluid didn’t seem very clear but sufficient to finish our lab on time. 2.) Add 20ml of dichloromethane, gently shake to extract, be sure to vent by opening the stop-cock. First extraction successful. 3.) Let
Next, I poured distilled water just below the 250ml mark on the neck of the volumetric flask.
8. Repeat step 7 with H2SO4, except that you should use a 10 mL graduated cylinder of H2SO4 and adding 15 mL water.
Method: Distillation is based on the fact that the matter can exist in three phases - - solid, liquid and gas. As the temperature of a pure substance is increased, it passes through these phases, making a transition at a specific temperature from solid to liquid (melting point--mp) and then at a higher temperature from liquid to gas (boiling point--bp). Distillation involves evaporating a liquid into a gas phase, then condensing the gas back into a liquid and collecting the liquid in a clean receiver. Substances that have a higher boiling point than the desired material will not distill at the
Fill a test tube about 1/3 full with cold tap water for use in step 34.
With a 9-inch pipet was used to add water through the condenser to keep the flask no more than half way full. Clove oil was extracted from the distillate in 1 mL increments every 5 to 10 minutes. The distillation and extraction process was approximately 37 minutes with 7 mL of distillate recovered. The product recovered was a light yellow liquid color with the same strong, sweet, cinnamon odor as the raw clove. 1 mL of dichloromethane solution was used to rinse the Hickman still and was then transferred to the centrifuge tube. Another 2 mL more of dichloromethane was added and shaken vigorously. Upon shaking the the mixture turned a cloudy white color with two layers resulting. The major component of clove oil was extracted with two more 3 mL portions of dichloromethane solution. The mixture was allowed to cool and left in the hood overnight to dry.
Distillation of the first product began at 83 °C. A Pasteur pipette was used to remove 1-ml of the distillate into a vial. A second vial was filled with distillate until it reached 1-ml. As the second vial is being filled, observe the temperature and remove the apparatus from the heat source if there is an observed drop in temperature.
Distillation. Transfer the clear liquid to a dry 25-mL round-bottom flask using a Pasteur pipet. Add a boiling stone and distill the crude t-pentyl chloride in a dry apparatus. Collect the pure t-pentyl chloride in a receiver cooled in ice. Collect the material that boils between 78°C and 84°C. Weigh the product and calculate the percentage yield.
Simple distillation is a separation technique which can be used to separate and purify distillates from a liquid mixture which ideally contains one volatile and one non-volatile compound. If such ideal conditions are not possible—as is usually the case—then simple distillation can be applied as long as the liquid in question is composed of compounds that differ in volatility such that their boiling points differ by at least 40 to 50 degrees Celsius. Because
XII. Take the 250 ml beaker to your lab bench. Set up a gravity filtration with a plastic funnel, folded wet filter paper, and an Erlenmeyer flask. Pour the content in the 250 ml beaker slowly through the filter paper. Wash the filter paper with deionized water. Dispose of the filtrate in the proper labeled waste container.
1) Separate the solid from the liquid in the beaker by decanting the liquid. Ask your instructor to demonstrate the correct procedure.
Distillation is a method of separating two volatile chemicals on the basis of their differing boiling points. During this lab, students were given 30 mL of an unknown solution containing two colorless chemicals. Because the chemicals may have had a relatively close boiling point, we had to employ a fractional distillation over a simple distillation. By adding a fractionating column between the boiling flask and the condenser, we were able to separate the liquids more efficiently due to the fact that more volatile liquids tend to push towards the top of the fractionating column, thereby leaving the liquid with the lower boiling point towards the bottom. After obtaining the distillates, we utilized a gas chromatograph in order to analyze the volatile substances in the gas phase and determine their composition percentage of the initial solution. Overall, through this lab we were able to enhance our knowledge on the practical utilization of chemical theories, and thus also demonstrated technical fluency involving the equipment.
Distillation is a wide-range laboratory technique used to separate and purify liquids based on the differences between their conditions.1 Mixtures of liquids with different boiling points are heated
Today marks the 27th day of the distillation process. It seems like just yesterday that I made my first six papers in the process. However, there are now 156 black, white and ochre papers stacked up high on my studio table that tells me otherwise. The papers crackle as I stack and smooth them at the beginning of each day. The process begins as I take down the previous days finished papers and put them in the stack before I begin again. I tape one paper on my painting wall, work on it until completion and then move it to the side and back wall to dry. Each day the walls get covered with six more wet and almost tattered papers. The thin paper dries and warps at the edges, it folds, gathers, and at times looks like fabric from the paint water. The left behind tape on the corners and at times hidden under a layer of paint to cover tears and rips in the paper hints at the process. I love
3. Use a sterile pipette to transfer 0.1 ml of each dilution on to a MacConkey agar plate.
Distillation is a technique used for separating, identifying and purifying liquids. Simple Distillation and fractional distillation are often used for isolation of mixture of liquids. In this experiment, steam distillation is used to separate carvone from caraway seeds and spearmint leaves. For steam distillation, the bp has to be less than 100° C, compound mixed with water has to be stable at 100° C.The principles of steam distillation focus on Raoult’s law and Dalton’s law. However, since it is not soluble in water, it does not depend on its mole fraction in the mixture. Therefore, Raoult’s law does not apply to steam distillation because the compounds are immiscible, so they do not depend on each other’s mole fraction. According to Dalton’s law total vapor pressure is higher than most volatile component and boiling point mixture is lower