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Chemistry Laboratory BKF 2711

LABORATORY REPORT FRONTPAGE

CHEMISTRY LABORATORY (BKF2711) 2010/2011 Semester I


Title of Experiment Date of Experiment Date of Submission Instructors Name Group of Member Name 1. JESSLYN TAN KIM EAN 2. KHAIRUL ABIDIN BIN GHAZALI 3. ZULHILMI BIN KHAMIS 4. CHAN WILLIAM 5. LIM JIA HAN Group No. Section Marks : :2 : K33 Part A Part B TOTAL 55 45 100 : Extraction with Solvent : 13/08/10 : 20/08/10 : En.Khairil Anuar,Cik Rohana,En.Wan Ruzlan : ID KA10023 KA10032 KA10035 KA10038 KA10041

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Chemistry Laboratory BKF 2711 FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING Bil . 1. 2. 3. 4. 5. 6. 7. Abstract Introduction And Literature Review Experiment Objective Methodology Results And Discussion Conclusion And Recommendation Reference UNIVERSITI MALAYSIA PAHANG Contents Page 3 4-6 7 7-8 9 10 10

Table of Contents

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Chemistry Laboratory BKF 2711

Abstract The title of this experiment is extraction with solvents. The objective of the experiment is to demonstrate the effectiveness of a single extraction with a fixed volume of solvent compared to two extractions, each with one half of the fixed volume. During the experiment, the sample crystal violet, C25N3H30Cl was mixed with organic solvent, dichloromethane (CH 2Cl2). The sample was shaken with dichloromethane in a separatory funnel, left to stand undisturbed for a few minutes. Later, the lower part of the layer, which is dichloromethane was drawn off. The top part, an aqueous layer is transferred to a test tube. The procedure was repeated with using half of the initial volume of the dichloromethane to extract the sample and this step was repeated twice. From the result of the experiment, the sample crystal violet turned from violet to almost colourless. This shows that the solvent dichloromethane has managed to extract parts of the crystal violet. After comparison, we found out that the second sample is clearer than the first sample. From our observation, we can conclude that multiple extractions are more efficient compared to simple extraction. There were a few precautions for this experiment. Dichloromethane is a carcinogen which can cause cancer, hence minimize the expose of it. The second precaution is after the separatory funnel is shaken, the lower part of the funnel is open and pressure is released, this them must be handled with care as the gas released is in high pressure and it is dangerous.

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Chemistry Laboratory BKF 2711

Introduction Solvent extraction is an application of the Partition Law. Partition Law is a law used to explain the dynamic equilibrium of the distribution of a solute when mixed with two immiscible solvents. The law states that if a solute, X (solid or liquid) is added to a mixture of two immiscible liquids, it will distribute itself between the two liquids according to the partition law and in such a way that the ratio of the concentrations of the solute in the two solvents is a constant at a fixed temperature.

Concentration of X in solvent A = k (a constant) Concentration of X in solvent B The law holds only under certain conditions. The conditions are: a) The temperature must be constant. b) The solute is in the same molecular state in both solvents. c) The solute must not react, associate, or dissociate in both solvents. d) The two solutions must be reasonably dilute. e) The solvents are immiscible and do not react with each other. For solvent extraction, the knowledge of knowing that organic compounds are more soluble in organic solvents such as ethoxyethane(ether) and trichloromethane(chloroform) than in water and organic solvents are immiscible with water helps to enhance the process. These organic compounds can be extracted from aqueous solutions or suspensions by adding organic solvent, shaking, and separating the two layers in a separating funnel. The product is thus removed from

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Chemistry Laboratory BKF 2711

inorganic impurities which are soluble in water and the pure organic compound can then be obtained by distilling off the solvent. A good solvent should have the following properties: a) Solvent must be insoluble in water (to prevent dissociation or association of molecules) b) It must have high solubility for organic compounds. c) It must have a low boiling point so that it can be easily evaporated without using a high temperature. d) It must be chemically not reactive with most organic compounds. Solvent extraction is more efficient by using the given solvent in two or three batches rather than all at one time. Through this method, more of the product is recovered.

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Chemistry Laboratory BKF 2711

Literature Review This experiment is using the principle of solvent extraction. In this experiment, the solvent used is dichloromethane while the sample being extracted is crystal violet, C 25N3H30Cl During the experiment, 10mL of the sample is mixed with 10mL dichloromethane in a separatory funnel. Then, the mixture is shaken slowly. During the shaking process, the stopper should be opened from time to time to release the pressure released due to mixing of the two solutions. After that, the separatory funnel is left to stand. . The density of dichloromethane is higher than crystal violet. Therefore, when the two layers appear, the lower layer is dichloromethane while the upper layer is crystal violet. The lower layer is transferred out while the upper layer is transferred into a test tube. The process is repeated again, but this time the volume of solvent used is half and it is being used twice. The sample is mixed with 5mL dichloromethane and shaken slowly. Then, it is left to stand. The lower layer is then transferred out and the crystal violet is again mixed with 5mL dichloromethane. The same process of leaving it to stand and separating is again repeated. From our observation, the solvent dichloromethane experienced a change of colour from colourless to violet. As for the crystal violet, it turned from violet to colourless. However, the intensity of the first sample is darker than the intensity of the second sample. This denotes that the solvent extraction is more efficient if used in more batches rather than single batch.

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Chemistry Laboratory BKF 2711

Experiment Objective 1. To demonstrate the effectiveness of a single extraction with a fixed volume of solvent compared to two extractions, each with one half of the fixed volume. Methodology Equipment/Apparatus 10mL crystal violet, 125mL separatory funnel, 10mL of dichloromethane, rubber stopper, ring stand, Erlenmeyer flask

Procedures A. Simple Extraction The purpose of this experiment is to demonstrate the effectiveness of a single extraction with a fixed volume of solvent compared to two extractions, each with one half of the fixed volume. An aqueous solution of an intensely purple colored dye, crystal violet, will be extracted by dichloromethane (CH2Cl2) in which the dye is somewhat more soluble. The experiment is written for use of a separatory funnel, but it can be done effectively on one-fifth scale using the squirting technique. 1. 10 ml of the stock aqueous solution of crystal violet is placed in a 125 ml separatory funnel and is extracted with 10 ml of dichloromethane in the following manner. 2. 3. The separatory funnel is stopppered, shook gently, and is turned upside down. While the separatory funnel is in position, the stopcock is opened to release the internal pressure, the stopcock is closed, shook vigorously and the internal pressure in released again. 4. 5. This procedure is repeated four or five times, then the separatory funnel is supported upright in the ring and let it stand undisturbed. When the liquids have separated completely, the lower dichloromethane layer is drawn off into an Erlenmeyer flask.

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Chemistry Laboratory BKF 2711

6.

A portion of the remaining aqueous layer is transferred to a test tube and sited aside for later comparison.

Caution: Do not point the stem of funnel at anyone when you release the pressure. Any liquid in the stem may be ejected forcefully. Caution: Prolonged exposure to high concentrations of dichloromethane vapors may induce cancer. As with all organic solvents, it should be used in a well-ventilated area. B. Multiple Extractions 1. The separatory funnel is cleaned well with water and a second 10 ml portion of the stock solution of crystal violet is placed in it. 2. The solution is extracted with 5 ml of dichloromethane as described in part 1. The dichloromethane layer is drawn off into the Erlenmeyer flask used in part 1 and the remaining aqueous layer is extracted with a second, fresh 5 ml portion of dichloromethane. 3. The dichloromethane is drawn off into Erlenmeyer flask and transfer a portion of the aqueous layer is transferred into a test tube of the same size used in part 1. 4. Both tubes are filled to the same height. The effectiveness if extraction is compared by the two different procedures by noting the intensity of colour remaining in the aqueous layer.

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Chemistry Laboratory BKF 2711

Results and Discussion Results A. Simple Extraction 1. Two layers are formed after few minutes. 2. The lower layer is a solvent(dichloromethane) 3. The upper layer is a crystal violet solution. 4. Colour intensity of simple extraction is darker than multiple extraction. B. Multiple Extraction 1. Two layer are formed after few minutes. 2. After drawing out the lower dichloromethane layer and the addition of dichloromethane, two layers are formed again after a few minutes. 3. Colour intensity of multiple extraction is lighter than the simple extraction.

Discussion 1. Write the chemical equations for any reactions involved. C25N3H30Cl (aq) C25N3H30Cl (org) 2. What properties do you look for in a good solvent for extraction? A good solvent for extraction is immiscible with water (low solubility). The solvent have polarity and H-bonding for good recovery of analytes (organic phase). Solvents usually have a low boiling point and evaporate easily or can be removed by distillation, thereby leaving the dissolved substance behind after extraction (pre-concentration if necessary). Besides, a good solvent should be chemically inert.

Multiple extraction is more efficient than single extraction as it can increase the extraction yield. More analyte is extracted with multiple portions of extracting solvent than single portion of an equivalent volume of the extracting phase.

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Chemistry Laboratory BKF 2711

Conclusion Based on the result, we can conclude that the two extraction is more effectiveness compare to the single extraction with a fixed volume of solvent. During the experiment, should not point the steam of funnel at anyone when released the pressure because any liquid in the stem may be ejected forcefully. Prolonged exposure to high concentrations of dichloromethane vapors may induce cancer. As with all organic solvents, it should be used in a well-ventilated area.

References
Introduction to Organic Laboratory Techniques: A Small-Scale Approach by Donald L.Pavia Science 2004. Experimental Organic Chemistry A Small-Scale Approach by Charles F.Wilcox,Jr and Mary F.Wilcox 2nd Edition. Umland and Bellama (1999). General Chemistry. 3rd ed. Pacific Grove, CA: Brooks/Cole Publishing Company Chang, Raymond (2007). Chemistry.3rd ed. New York: McGraw-Hill

Tan Yin Toon, Kathirasan Muniandy, Loh Wai Leng(2008), Ace Ahead Chemistry Volume 1.Selangor: Oxford Fajar

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