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Methods of Purification and

Analysis

By the end of the lesson, you should be able to:

□ Describe chromatography and interpret a chromatogram.
□ Describe in general the use of locating agents.
□ Describe filtration.
□ Describe crystallisation.
□ Describe distillation.
□ Describe fractional distillation, examples: crude oil; ethanol from
fermentation.
□ Describe how the purity of substances can be tested using boiling point,
melting point and chromatography.
□ Explain the need for pure substances in everyday life.
□ Suggest a suitable method for separating a mixture to obtain pure
componenets.
□ Use Rf values to identify substances on chromatograms.

Please tick in the box if you can do any of the above.

The Need for Pure Substances

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 Many industries need pure substances to make products such as foods,
steel, computer chips and medicines.
⇒ What is pure substance?
A pure substance is a single substance not mixed with anything
else. E.g. white sugar or copper(II) sulphate crystals.

 In nature, very few substances are pure. Most substances are impure
and in the form of mixtures.
⇒ What is a mixture? Give an example of a mixture.
A mixture contains two or more substances. E.g. seawater as it
contains water, salt and other dissolved solids.

Obtaining Pure Substances

 Mixtures can be easily separated into pure substances. This process is
called purification.

 It is done by using physical methods WITHOUT chemical reactions.

Filtration

⇒ What is it used for?
This is used to separate a liquid from a solid.

⇒ What happens in the process?
- The method is shown in the diagram above.

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Salt in sea water cannot be separated from the water by filtration. What do you call this solid? residue . but the bits of solid are too large to go through the pores. The liquid goes through the filter paper.. ⇒ What are the main uses for filtration? Used to purify drinking water by removing insoluble solids. The dyes in ink go through filter paper. What do you call this liquid? Filtrate ⇒ How does the process work? . Why? Because the dye molecules are smaller than the pores in the paper and so go straight through them. 2. Crystallisation ⇒ What is it used for? 3 .The filter paper has holes in it called pores. The particles of liquid are small enough to go through the pores. Why? Because the sodium and chloride ions are much smaller than the pores in the paper. Quick Questions: 1. The solid is trapped by the filter paper.

. The liquid is boiled until much of the water has been evaporated. Use to separate a dissolved solid from a solution as well-formed crystals. ⇒ What are the main uses for crystallisation? To obtain pure sugar from sugar cane water. ⇒ What happens in the process? .So when the solution cools. Crystals form on cooling.The water is evaporated to make the hot solution saturated. The solution is put into an evaporating basin and heated. These can be filtered off and dried by pressing them between sheets of filter paper. . . Sublimation ⇒ What is it used for? Separates a mixture of solids. NOTES: Some water must usually be left when aqueous solutions of salts are being crystallized as the salt crystals need water of crystallization. ⇒ What happens in the process? 4 . ⇒ How does the process work? . . . . The hot solution is allowed to cool. one of which sublimes.A hot solution can dissolve more solid than a cold one. a lot of solid must come out of the solution as crystals. This means it can no longer dissolve any extra solid.

.The solute has a high melting and boiling point and so does not boil and remains in the flask. - ⇒ How does the process work? . NOTES: As only a few solids sublime.The solvent has a low boiling point and so is easily changed into a gas on heating. The solvent turns into a vapour and leaves the flask. this method of separation is limited. called the distillate. which changes it back into liquid. ⇒ What are the main uses for simple distillation? 5 . If a mixture of iodine and sand is heated in a beaker. The vapour changes back to solid directly on a cold surface. . the iodine changes from solid to vapour directly. . . ⇒ What happens in the process? . Simple Distillation ⇒ What is it used for? Use to separate a liquid from a solution of a solid.It is then cooled by a condenser. The sand is not affected by the heat and remains in the beaker.The solution boils. The solid is called the solute and the liquid is called the solvent.The solution is heated in a flask as shown in the diagram. . .

3. 2. Fractional Distillation ⇒ What is it used for? 6 . 4. Why do you think the condenser slopes downwards? So that the pure solvent can run into the receiver. Where is the bulb of the thermometer placed? It is placed beside the side arm of the distillation flask. Quick Questions: 1. Where does the water enter and leave the condenser? Enter from the bottom of the condenser and leave from the top. Why is it important that the thermometer does not dipped into the solution? This ensures that the thermometer measures the boiling point of the substance that is being distilled. Why do we not let it flow in the opposite direction? This is to ensure that the whole condenser is cold enough to collect the distillate. 5. Use to extract sodium chloride from sea water.

1.The mixture of liquids is heated in the flask as shown in the diagram. the fractionating column makes the high boiling point liquids condense and return to the flask. What do you call this liquid? distillate .It is then cooled by a condenser. allowing the lowest boiling point liquid to remain as a gas and escape. Quick Questions:  The thermometer shows a constant temperature during the distillation as pure liquid is being distilled as can be seen from the graph above.To separate substances in crude oil. What would be temperature while ethanol is distilled? 7 .The liquids must have different boiling points. When a mixture of ethanol and water is being distilled. .When the mixture of the liquids boil. . The liquid with the lowest boiling point comes out of the top of the fractionating column.The mixture boils. (They are said to be miscible) ⇒ What happens in the process? . which changes back into liquid. . . which one will be distilled first? Ethanol 2. ⇒ What are the main uses for fractional distillation? . the liquid with the next lowest boiling point is then distilled.After most of the first liquid has distilled.To separate gases from liquid air. ⇒ How does the process work? .To separate a mixture of two or more liquids which mix completely with one another.

. Use of a Separating Funnel -Liquids that do not mix with each other are said to be immiscible liquids.The oil and water form two separate layers. with the less dense liquid being on top.The mixture is placed in a separating funnel and allowed to stand.78°C 3. When will the temperature increases to 100°C? When all the ethanol has been distilled. such as oil and water. . Determining Purity  There are 3 methods to determine the purity of a substance: a) By chromatography b) By boiling point c) By melting point a) By chromatography  What is the main use of chromatography? 8 . can be separated by using a separating funnel.

Chromatogram 1 chromatogram 2  How would you interpret chromatogram 1 and chromatogram 2? Chromatogram 1: It shows that the spot of green food colouring is a mixture of two dyes because there are two spots on the chromatogram. Chromatogram 2: It shows that the substance is pure because it is only made up of only one dye. .The more soluble the substance the faster it will dissolve in the solvent.  How does chromatography work? The substance in the mixture dissolves in the solvent and move up the paper.Use to separate and identify mixtures of substances. . 9 . Rf values  Substances on chromatograms can be identified by their Rf value.The more soluble substance will get carried along faster by the solvent and move further ahead of the less soluble solutes. It is also use to analyse whether a substance is pure or not. They become spread out as each substance moves at a different speed.  What is a chromatogram? It is the chromatography paper with the separated components .  Why do certain spots move further away from the others? .Different substances have different solubilities in the same solvent. such as coloured dyes in inks and food.

Rf value = distance moved by substance on the paper Distance moved by the solvent A B ⇒ Calculate the Rf value for chromatogram A and B.  A substance can be identified by .looking up its Rf value in a reference book.  Each substance has a particular Rf value for a given solvent. chromatography can also be use to analyse colourless substances. Experiment on Chromatography 10 . chromatography paper and temperature. However.  Most of the time. . ⇒ How do we perform chromatography on colourless substances? By applying a locating agent on the chromatogram. chromatography is used to separate coloured substances.Finding a known spot on the chromatogram at exactly the same height as it must also have the same Rf value.

c)Pour about 1 cm of ethanol in the beaker. the following instructions were given.Aim of experiment: To separate and identify the different compounds in green ink using paper chromatography. 1) The starting line should be drawn with a pencil rather than with ink. b)Place a drop of fine ink on the pencil line. the solvent front should be near the 11 . f) Remove the paper when the solvent has almost reached the top of the paper. e) Leave it to develop. it will interfere with the chromatogram. g) Allow the paper to dry and paste it in the space above. Cover the beaker with a lid. Result: List the colours seen in the paper _______________________________________________________ Conclusion: What can you conclude from this experiment? _______________________________________________________ _______________________________________________________ Follow-up Questions: In preparing the chromatogram. Procedure: a)Draw a starting line in the chromatography paper about 2 cm using pencil. Suggest a reason for each instruction. 2) At the end of the experiment. Because ink is a mixture of dyes and therefore if used for drawing the starting line. d) Lower the paper into the beaker containing the ethanol until the spots of ink are just above the surface of the solvent.

To ensure that all the mixture are separated. Add two or three boiling chips into the liquid to ensure smooth boiling. 4) The beaker is closed with a lid. This is to avoid smudging of the dyes that can affect the separation of the mixtures.top of the paper. To avoid the evaporation of the solvent. The setup use for the experiment to determine the boiling point of a substance. 12 . Pour 10 cm3 of propanone into a small distillation flask. 5) The starting line must be above the solvent To prevent the chemicals in the spot from dissolving into the main solvent solution. 3) The spots of the solutions and dyes on the starting line should be small. Procedure: 1. b) By boiling point Experiment on boiling point Aim of experiment: To study the effect of an impurity on the boiling point of propanone.

13 . 4. Can its boiling point be determined by using the apparatus in this experiment? State and explain TWO changes that would be necessary in Figure 2 in order to determine the boiling point of ethylbenzene.2. 5. 4. What are the effects of the alcohol on the boiling point of propanone? The boiling point will increase. 3. The greater the amount of impurities.Why must the water not heated too quickly? By heating it quickly. the boiling point might be missed or overlooked. What is the boiling point of a) pure propanone 56°C b) propanone containing alcohol? 2. Ethylbenzene has a boiling point of 136°C. Clamp the small distillation flask in a beaker half-filled with water and fix the thermometer so that the bulb is situated at the side outlet tube. 3. Follow-up questions: 1. Repeat the experiment with a mixture containing propanone and alcohol Results: Plot two graphs of time against temperature by showing clearly the main difference between the boiling point of pure propanone and impure propanone. Record the temperature when the liquid boils.Heat the water gently while stirring continuously. The liquid will boil over a range of temperature. the higher the boiling point.

Record the temperature when the solid melts. Results: Plot two graphs of time against temperature by showing clearly the main difference between the melting point of pure benzoic acid and impure benzoic acid. Procedure: 1. 4.1) The water bath should be change using a liquid which is higher than the boiling point of ethylbenzene. Secure the tube to the thermometer with a rubber band and place them in a small beaker containing paraffin oil. By melting point Experiment on melting point Aim of experiment: To study the effect of an impurity on the melting point of benzoic acid The setup use for the experiment to determine the melting point of a substance. 2) The thermometer should be change to a thermometer which has a higher temperature range. Repeat the experiment using a mixture containing benzoic acid and a small amount of naphthalene as the impurity. 2. 14 . Put a small amount of pure solid benzoic acid into a melting point. 3. Heat the oil slowly while stirring continuously.

contaminated with harmful substances can cause adverse side-effects in the human body and in extreme cases.e. The importance of purity in substances  Foodstuffs that are impure i. The greater the amount of impurities.  Drugs that are impure can cause adverse allergic reactions that may lead to death. 4.  Pure copper is needed to make copper wire used in electrical wiring. What is the melting point of a) pure benzoic acid 122°C b) benzoic acid contaminated with naphthalene? 118-121°C 2. State the effect of the impurity on the melting point of benzoic acid.  Pure silicon is used to make silicon chips for making microprocessors. the boiling point of benzoic acid will not be able to be reach since water will boil at 100°C. the lower the melting point 3. Why must a stirrer be used? To ensure equal distribution of heat throughout the liquid. The substance will melt over a range of temperature. Suggest why paraffin is used instead of water in this experiment. may even lead to death. 15 . By using water.Follow-up questions: 1. The melting point will decrease.

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