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Chemistry Laboratory

BKF 2711

LABORATORY REPORT FRONTPAGE

CHEMISTRY LABORATORY
(BKF2711)
2010/2011 Semester I

Title of Experiment : Extraction with Solvent

Date of Experiment : 13/08/10

Date of Submission : 20/08/10

Instructors Name : En.Khairil Anuar,Cik Rohana,En.Wan Ruzlan

Group of Member :

Name ID

1. JESSLYN TAN KIM EAN KA10023

2. KHAIRUL ABIDIN BIN GHAZALI KA10032

3. ZULHILMI BIN KHAMIS KA10035

4. CHAN WILLIAM KA10038

5. LIM JIA HAN KA10041

Group No. :2
Section : K33
Marks Part A 55 :

Part B 45

TOTAL 100

FACULTY OF CHEMICAL AND NATURAL RESOURCES ENGINEERING

UNIVERSITI MALAYSIA PAHANG

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Bil. Contents Page

1. Abstract 3

2. Introduction And Literature Review 4-6

3. Experiment Objective 7

4. Methodology 7-8

5. Results And Discussion 9

6. Conclusion And Recommendation 10

7. Reference 10

Table of Contents

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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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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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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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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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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. The separatory funnel is stopppered, shook gently, and is turned upside down.
3. 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. This procedure is repeated four or five times, then the separatory funnel is
supported upright in the ring and let it stand undisturbed.
5. When the liquids have separated completely, the lower dichloromethane layer is
drawn off into an Erlenmeyer flask.

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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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Results and Discussion

Results

A. Simple Extraction B. Multiple Extraction

1. Two layers are formed after few minutes. 1. Two layer are formed after few minutes.

2. The lower layer is a 2. After drawing out the lower


solvent(dichloromethane) dichloromethane layer and the addition of

3. The upper layer is a crystal violet solution. dichloromethane, two layers are formed again
after a few minutes.

4. Colour intensity of simple extraction is 3. Colour intensity of multiple extraction is


darker than multiple extraction. 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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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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