Reflux Ring Lab Report

The purpose of this lab is to separate a mixture and determine the percentages of each of the ingredients. Each substance will have a different boiling point due to its intrinsic properties and from that, we will be able to determine the purity of different products as we evaporate off the next level of product.

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.

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

This is called refluxing, where the liquid is condensed and returned to liquid. [1] There are many real life applications of distillation that are used everyday,

This was done by using common lab method known as simple distillation, which is used to separate a volatile liquid from a non-volatile liquid, and also to separate two liquids that have boiling point differences of above 50 oC. The boiling point of any liquid is obtained when the total pressure above the liquid is equal to the atmospheric pressure. Other objective of this experiment was to learn how to use the Gas Chromatography to check whether the two components in a mixture successfully separated. The results of the calculated GC percent composition indicate that the two components were not successfully separated by simple distillation, but it was very close to the calculated percentage composition. This may be because the boiling points of the ethyl acetate (77.1 oC) and butyl acetate (126 oC) are not that far apart, and simple distillation shows positive results if the two liquids boiling points differ by greater than 50 oC. The second reason could be that enough fractions were not used.

Product was rinsed/washed with separate 5 mL portions of ice-cold ethanol. Appearance was recorded of the solid and filtrate before liquid was discarded. Product was dried for 24 hours by being placed in the dark.

The purpose of this step was to further purify the ester and remove any impurities that may have still remained after the purification in the previous steps. The organic ester layer was then added to a small quick fit flask wherein crushed anhydrous calcium chloride was added. Anhydrous calcium chloride is a drying agent that removes polar compounds by fusing with them. As water is polar and the ester, butyl-ethanote, is not very polar, the anhydrous calcium chloride fused only with any traces of water that may have still been present in the mixture, absorbing them, and therefore, removing them from the ester. To check whether all, or a majority of the water particles had been absorbed, the flask was swirled to see if the anhydrous calcium chloride was clumping anywhere in mixture. If clumping occurred, it meant that it was still fusing with and absorbing water particles and that they had not yet been removed. Once the calcium chloride powder began to flow freely, it was an indicator that most of the water particles had been absorbed. However, to ensure that the ester would be as pure as possible, the anhydrous calcium chloride was left to fuse and absorb the water overnight so that as many water particles could be removed as

2. Why is the mixture extracted with sodium bicarbonate? Give an equation and explain its relevance.

The organic solution was washed with water by adding 2 separate 20cm3of water and filtering water out after each addition. Then 2 further separate additions of brine measuring 20cm3each and again filtering brine to retain only the organic solution. Magnesium sulphate dried the organic solution and filtered into a pre-weighed (66.24g) 100cm3round bottom flask to remove ethyl acetate with the rotary evaporator. A vacuum desiccator was used to dry the material for

In simple distillation, the distillate collected was not nearly as pure as Fractional distillation because Fractional distillation allows for additional distillation and purification of these liquid components due to the beads that act as theoretical plates. Also, in Simple Distillation, the boiling point of water was reached a littler earlier and this would have begun to

25 mL of chilled, distilled water were added to the reaction flask, and the crystal lumps in the flask were broken up with a stirring rod. A piece of filter paper was weighed, and the mass was recorded. The filter paper was placed in the Buchner funnel, and it was moistened with 1-2 mL of chilled, distilled water. A piece of pressure tubing was attached to the side arm of the filter flask and to a filter trap attached to a water aspirator. The aspirator was turned on to draw the water in the funnel into the flask and to seal the filter paper to the funnel.

However, if we were to proceed with Distillation first, we could elimate all contiante in the mix, as seen in the demonstration in Experiment 1. These would make the process of decantation, filtration, solvent extraction, adsorption redundant. In Nature: 439 (Martyn J, et al. 2006) it is said that;

The purpose of distillation is to purify a liquid. Distillations are use to purify contaminates out of water to obtain clean pure water, as well as, to separate mixtures of liquids into their individual components; e.g. methanol and water.

To determine the identity of the final product, it is significant to determine the Infrared bands of the starting material (3-nitroacetophenone). Infrared spectrum can help to gather information, asses the impurity as well as to identify the molecules present in a compound. In this experiment, student found out that all the functional groups present in a 3-nitroacetophenone molecule (NO2, OH, C=O, NH2) have polar bonds. These polar bonds when stretched give an increase to important molecular dipole changes and therefore illustrate an intense IR

Simple distillation can be effective if the different substances have a fifty or more degree distinction in their boiling points. In this generally a boiling flask is used with a thermometer to detect the boiling point of the substances. A condenser is attached that has cold water passing continuously which then leads to another flask that contains the purified liquid. A liquid is boiled into a vapor which is then concentrated back into a liquid form. This process happens to be a very common form of purifying organic liquids. An organic liquid is a compound containing