Topics Pure Substances & Mixtures Parameters of Purification Techniques of Purification Importance of Analysis Pure Substances A Pure Substance contains Only one substance One type of atom or molecule No contaminating impurities Mixtures Mixtures are formed by a physical change Separated by methods of purification
Parameters of Purification A pure substance has a fixed and definite melting and boiling point. Precise & predictable Can be used to test the purity of a sample A pure substance has a fixed solubility Solubility curve Chromatogram A pure substance has physical properties which are EXACT, PRECISE, DEFINITE & PREDICTABLE Parameters of Purification The presence of an impurity in a substance Lowers the melting point Raises the boiling point of a substance Changes will be spread over a range of temperatures Sharpness at a particular point will not be observed Methods of Purification Mixture Type Method Solid + Solid Soluble & Insoluble Filtration & Decantation Solid + Solid Soluble Chromatography Solid + Liquid Insoluble Solid Filtration Centrifugation Decantation Solid + Liquid Soluble Solid Evaporation Crystalization Distillation Liquid + Liquid Immiscible Using a Separating Funnel Liquid + Liquid Miscible Fractional Distillation Separating Mixtures Decantation solid insoluble particles from a liquid (set, particles settle and pour off liquid)
Separating Mixtures Filtration solid insoluble particles from a liquid
Filtration Used to separate heterogeneous mixtures composed of solids and liquids Uses a porous barrier to separate the solid from the liquid Liquid passes through leaving the solid in the filter paper Filtration Gravity Filtration This is the simplest kind of filtration when the solution to be filtered is poured through a filter paper in a filter funnel. The filtration of hot solutions through a heated funnel and fluted filter paper is often carried out as part of a recrystallisation. Gravity filtration is generally carried out to remove impurities rather than to isolate solids. Buchner Filtration When a solid needs to be isolated from a solution it is normally done at a reduced pressure using a Buchner flask and Buchner funnel. Separating Mixtures Distillation a way of obtaining a pure solvent from a solution (boil, evaporation : steam, cooled : condenses, solvent is collected in another vessel)
Distillation Used to separate homogeneous mixtures Based on differences in boiling points of substances involved solution boiled in distilling flask and vapour/steam cooled and condensed in a Liebig condenser condenser consists of jacket of cold water with coldest water entering bottom of jacket and circulating out through the top ensuring that coldest part of condenser is just before the vapour escapes and that the jacket is completly full of water condensed solvent distillate all impurities left in distilling flask Simple vs Fractional Distillation Simple distillation is used to separate solvent from a non-volatile solute (i.e. solute with high boiling point). Eg. Water from salt solution. Fractional distillation is used to separate mixture of miscible liquids, eg. Mixture of ethanol and water.
Fractional Distillation How fractionating column works May be filled with glass beads, plates or a spiral. These provide a large surface area for vapour to condense on. Liquid with lowest boiling point will distill over to the condenser first Vapours of liquids with higher boiling points condense along fractionating column and re- enters the round-bottomed flask
Fractional Distillation Fractional Distillation Industrial Applications oil refineries separating the various components of crude oil or petroleum Sublimation process used to separate a solid that sublimes from one that does not Eg: mixture of iodine + copper; mixture of ammonium chloride + sodium chloride When a mixture of a solid that sublimes and a solid that does not is heated, the solid that sublimes will turn into a vapour and separates from the other solid which remains in the container. Sublimation Evaporation can be used to separate a solute from the solvent in a solution.
Only for solids that will NOT decompose on heating.
Eg. sodium chloride (common salt) from salt solution A separating funnel can be used to separate two liquids which are immiscible, For eg. Oil & Water Chromatography Separates components of a mixture based on ability of each component to be drawn across the surface of another material and based on their solubility Mixture is usually liquid and is usually drawn across chromatography paper Separation occurs because various components travel at different rates Components with strongest attraction for paper travel the least and components with the highest solubility travel the most Important Concepts in Paper Chromatography Capillary Action the movement of liquid within the spaces of a porous material due to the forces of adhesion, cohesion, and surface tension. The liquid is able to move up the filter paper because its attraction to itself is stronger than the force of gravity.
Solubility the degree to which a material (solute) dissolves into a solvent. Solutes dissolve into solvents that have similar properties. (Like dissolves like) This allows different solutes to be separated by different combinations of solvents.
Separation of components depends on both their solubility in the mobile phase and their differential affinity to the mobile phase and the stationary phase. Simple Example of Paper Chromatography using Marker Pens
Chromatography Examples of Chromatography
Gas Chromatography Used to determine the chemical composition of unknown substances, such as the different compounds in gasoline shown by each separate peak in the graph below. Paper Chromatography Can be used to separate the components of inks, dyes, plant compounds (chlorophyll), make- up, and many other substances Liquid Chromatography Used to identify unknown plant pigments & other compounds. Thin-Layer Chromatography Uses thin plastic or glass trays to identify the composition of pigments, chemicals, and other unknown substances. What if the substances you are interested in are colourless? In some cases, it may be possible to make the spots visible by reacting them with something which produces a coloured product. A good example of this is in chromatograms produced from amino acid mixtures. Suppose you had a mixture of amino acids and wanted to find out which particular amino acids the mixture contained. For simplicity we'll assume that you know the mixture can only possibly contain five of the common amino acids.
What if the substances you are interested in are colourless? A small drop of a solution of the mixture is placed on the base line of the paper, and similar small spots of the known amino acids are placed alongside it. The paper is then stood in a suitable solvent and left to develop as before. In the diagram, the mixture is M, and the known amino acids are labelled 1 to 5. The position of the solvent front is marked in pencil and the chromatogram is allowed to dry and is then sprayed with a solution of ninhydrin. Ninhydrin reacts with amino acids to give coloured compounds, mainly brown or purple.
What if the substances you are interested in are colourless? The left-hand diagram shows the paper after the solvent front has almost reached the top. The spots are still invisible. The second diagram shows what it might look like after spraying with ninhydrin. What if the substances you are interested in are colourless? There is no need to measure the R f values because you can easily compare the spots in the mixture with those of the known amino acids - both from their positions and their colours. In this example, the mixture contains the amino acids labelled as 1, 4 and 5. And what if the mixture contained amino acids other than the ones we have used for comparison? There would be spots in the mixture which didn't match those from the known amino acids. You would have to re-run the experiment using other amino acids for comparison.
Chromatography - Applications analyzing ink dyes for forgery cases analyzing food dyes to ensure that only permitted colorings are used in foodstuffs checking whether pesticides on vegetables exceed safe levels detecting trace levels of drugs in urine samples separation of amino acids, proteins & carbohydrates. analysis of drugs, hormones, vitamins & brain amines. determination of molecular weight of proteins. isolation of plant pigments from roots and leaves.
Uses for Chromatography Chromatography is used by scientists to:
Analyze examine a mixture, its components, and their relations to one another Identify determine the identity of a mixture or components based on known components Purify separate components in order to isolate one of interest for further study Quantify determine the amount of the a mixture and/or the components present in the sample
Uses for Chromatography Real-life examples of uses for chromatography: Pharmaceutical Company determine amount of each chemical found in new product Hospital detect blood or alcohol levels in a patients blood stream Law Enforcement to compare a sample found at a crime scene to samples from suspects Environmental Agency determine the level of pollutants in the water supply Manufacturing Plant to purify a chemical needed to make a product R f Factor
Retention Factor It is a number that represents how far a compound travels in a particular solvent.
It is measured by measuring the ratio of the distance traveled by the compound and the distance traveled by the solvent.
Rf ( Retention Factor )Value distance traveled by component from application point Rf = ----------------------------------------------------------------------------- distance traveled by solvent from application point
R = zero, - Solute remains in the stationary phase and thus it is immobile. R = 1 - Solute has no affinity for the stationary phase and travels with the solvent front.
Separating Mixtures Centrifuging solid particles from a suspension (liquid spun very quickly in a centrifuge pushes particles to sides and liquid can poured or filtered off)