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Mixtures and their separations
Janadi Gonzalez-Lord
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Table of contents
•   Syllabus requirements
•   Pure and impure substances
•   Classification of mixtures
•   Separation of mixtures
•   Types of separation techniques
•   Experiments
•   Industrial uses
•   Separating mixtures in everyday life
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Syllabus requirements - Mixtures
a) differentiate between mixtures and compounds in terms of composition and formation

b) recognize that the components of mixtures can be separated by simple means

c) define the terms : miscible , immiscible , soluble , insoluble , heterogeneous , homogenous , and
   apply them correctly i.e. miscible refers to liquids , soluble to gases and solids

d) identify mixtures as solutions , suspensions , colloids , emulsions based on the states of matter
   present and their solubility / miscibility

e) define solute and solvent

f) identify dissolving as one substance fitting in between the spaces of another substance .

g) identify a method of separating mixtures based on their composition

h) describe the separating methods of simple distillation , fractional distillation , filtration , layer
   separation

i) draw line diagrams for the methods in (h)
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Syllabus requirements - Mixtures
j.   carry out filtration and layer separation in the laboratory and write up notes about the
     procedure and results

k. recognize that filtration separates particle based on size

l. Identify sieving , sifting and straining as everyday methods of filtration

m. observe the set up as a teacher demonstration the simple distillation process

n. identify other methods of separation such as chromatography , centrifugation , solvent extraction

o. suggest methods for separating mixtures based on the properties of their components e.g. sand
   and salt

p. name two industrial methods of separating mixtures e.g. fractional distillation used to obtained
   distilled spirits , centrifugation used to separate components of blood / body fluids in laboratory
   testing , filtration in purification of domestic water supply
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Matter can be sub-divided into PURE and IMPURE SUBSTANCES or MIXTURES.

PURE substances can be sub-divided into ELEMENTS and COMPOUNDS

IMPURE substances or MIXTURES can be sub-divided into HOMOGENOUS and
HETEROGENOUS
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                                                                 Can be separated into



                                                                                          Can be
Can be                                                                                    separated
separated                                                                                 into
into




 Source: www.mghs.sa.edu.au/Internet/Faculties/Science/Year10/Pics/elementsAndCompounds.gif
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Elements versus compounds
An element....                      A compound......
• consists of only one kind of      • consists of atoms of two or
  atom                                more different elements
• cannot be broken down into a        bound together,
  simpler type of matter by         • can be broken down into a
  either physical or chemical         simpler type of matter
  means                               (elements) by chemical means
• can exist as either atoms (e.g.     (but not by physical means),
  argon) or molecules               • has properties that are
  (e.g., nitrogen).                   different from its component
                                      elements,
                                    • always contains the same ratio
                                      of its component atoms
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                  An element
                  Consists of only one kind of atom
Ar
         Ar
                  can exist as either atoms (e.g. argon)

                  or molecules (e.g., nitrogen).

                  cannot be broken down into a simpler
                  type of matter by either physical or
                  chemical means

N    N            If you try to break apart an atom or
                  molecule, you get an ATOMIC BOMB




         N    N
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        H       H                               A compound
            O                                   consists of atoms of two or more
                                                different elements bound together

                                                always contains the same ratio of its
                                                component atoms
                    H           H
                            O                   Water (formula H2O)

                                                For every water molecule, there are 2
                                                Hydrogen atoms for every 1 Oxygen
H   H           O       O           H       H   atom
                                        O
                                                has properties that are different from its
                                    H       H   component elements
                                        O
                                                For example, hydrogen and oxygen are
                                                gases but water is a liquid
                                    H       H
                                        O
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Examples of elements and compounds

                                                                               Elements




                                                                              Compounds




Source: www.physicalgeography.net/fundamentals/images/compounds_molecules.jpg
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Compounds versus Mixtures
A mixture....                           Remember that a compound...
 • consists of two or more              • consists of atoms of two or
   different elements and/or              more different elements
   compounds physically                   bound together,
   intermingled                         • can be broken down into a
 • can be separated into its              simpler type of matter
   components by physical                 (elements) by chemical means
   means, and                             (but not by physical means),
 • often retains many of the            • has properties that are
   properties of its components.          different from its component
Syllabus requirement met:                 elements,
differentiate between mixtures and      • always contains the same ratio
compounds in terms of composition and     of its component atoms
formation
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A mixture can be...
                                                             A mixture of different
A mixture of different   A mixture of different
                                                              types of atoms and
   types of atoms          types of molecules
                                                                  molecules

                          N    N
                                                              N         N



                                   O    O




                          H    H
                                                                       H       H


                                   Cl   H
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Match the following
                 1.   Pure elements               Answer: A, C, D

                 2.   Elements made of SINGLE ATOMS
                                                  Answer: A, D
                 3.   An element made of MOLECULES
                                                  Answer: C
                 4.   Mixture of TWO elements
                                                  Answer: E, F
                 5.   Mixture of THREE elements
                                                  Answer: H
                 6.   Pure compounds              Answer: G

                 7.   Mixture of TWO compounds
                                                  Answer: B
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Mixtures can be......
Homogeneous                                 Heterogeneous
• The prefixes "homo"- indicate             • The prefixes: "hetero"-
  sameness                                    indicate difference.

• A homogeneous mixture has                 • A heterogeneous mixture
  the same uniform appearance                 consists of visibly different
  and composition throughout.                 substances or phases.

• Many homogeneous mixtures                 • The three phases or states of
  are commonly referred to as                 matter are gas, liquid, and
  solutions.                                  solid.
 Syllabus requirements met:
 define the terms : heterogeneous , homogenous and apply them correctly
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Example of homogeneous
mixtures
Some mixtures around us are things we
don't even think of as mixtures.

Vinegar is a homogeneous mixture of
water and acetic acid (CH3COOH).

Most commercial vinegars have an
acetic acid content of about 5%. Acetic
acid gives vinegar its characteristic odor.
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Example of heterogeneous
mixtures
The combination of oil and vinegar in
salad dressing is a common example of a
HETEROGENEOUS mixture.

Here the two layers are distinctly visible.

Each layer by itself is considered a
HOMOGENEOUS mixture.
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Mixtures can be same phase.....

               Liquid +
                Liquid
     Solid +                      Gas +
      Solid                        Gas

               Mixtures
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Or Mixtures can be mixed-phase

              Solid +
               Gas
    Solid +                  Liquid
    Liquid                   + Gas

              Mixtures
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                  Gas + Gas
                  • Example: Air (        Gas + Liquid
                    N2, O2 , Ar, CO2      • Example:
                    , other gases)          Carbonated
                                            beverages (CO2
 Liquid +                                   in water)
 Liquid
                                                                       Solid + Liquid
 • Example:
   gasoline (a                                                         • Example: Sea
   mixture of                                                            water ( NaCl and
   hydrocarbon                                                           other salts in
   compounds)                                                            water)




Solid +                                                                            Solid + Gas
Solid                                                                              • Example: H2 in
• Alloys –                         Homogeneous                                       platinum or
                                                                                     palladium
  mixtures of                        Mixtures
  metals
• Example :
  brass (Cu/Zn)
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                 Liquid + Liquid
                 • EMULSION             Solid + Liquid
                 • Example: milk
                                        • SUSPENSION: Examples:
                                          Tomato juice, jello, blood
                                        • COLLOIDS: Example:
                                          glue, paint


Solid + Solid                                                          Solid + Gas
• Example : Gravel
  (sand, clay and small                                                • Example: Smoke
  rocks)                                                                 (Air and carbon
                                                                         particles)
                                   Heterogeneous
                                     Mixtures
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Liquid-Liquid solutions
 Example:                                 Example:               Example:
 Oil and water                            Phenol and water       Ethanol and water



                                                 Partially
   Immiscible                                                            Miscible
                                                 miscible

Syllabus requirement met:
define the terms : miscible , immiscible , and
apply them correctly i.e. miscible refers to
liquids



                                  Increasing mixability
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                                                                         Syllabus requirement met:
                                                                         identify mixtures as solutions
                                                                         , suspensions , colloids , emulsions

Heterogeneous mixtures                                                   based on the states of matter present
                                                                         and their solubility / miscibility


Solute does not fully dissolve in   Solution <Solute particle         Liquid + liquid
solvent                             size< Suspension
                                                                      Will separate into
Solute particles are clearly        Solute particles do not           immiscible liquids ONLY if
visible                             settle out on standing            no stabiliser added

Solute particles settle out upon    Solute particles can pass
standing                            through filter paper



      Suspensions                     Colloids                      Emulsions


                         Increasing solute particle size
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Solutions
Solute              Solvent             Solution
                                                                    homogeneous
                                                                      mixture
                        substance in
   The substance
                         which the
   which is being
                          solute is
     dissolved
                         dissolved




                                         Syllabus requirement met:
                                         Define solute and solvent
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DECREASING SOLUBILITY
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Table salt dissolving in water
                                 Dissolving.

                                 When a solute dissolves in a
                                 solvent, the particles of the solute
                                 fit in between the particles of the
                                 solvent.

                                 There is no chemical reaction. The
                                 change is reversible and the
                                 essential components of the
                                 mixture remains the same.

                                           Syllabus requirement met:
                                           Identify dissolving as one
                                           substance fitting in between the
                                           spaces of another substance .
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A mixture of different
                                              Separate atoms and
 types of atoms and
                                                  molecules
     molecules


                                        N            N                   N   N


           O     O
                         Can be
                         separated by   O          O                     O   O
                         PHYSICAL
                         MEANS into
          N    N
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SUBLIMATION                                   SOLVENT
• One substance                               EXTRACTION
  sublimes, the other                         • Differing solubilities
  does not                                      in a particular solvent
• Example:                                    • Example: Iodine +
  Ammonium chloride                             sodium chloride
  + sodium chloride


                        Solid +
                         solid
                        mixtures
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FRACTIONAL                                   SEPARATING
DISTILLATION                                 FUNNEL
• Miscible                                   • Immiscible
• Slightly differing                         • Differing densities
  boiling points                             • Example: Oil + water
• Example: Ethanol +
  water



                       Liquid +
                        liquid
                       mixtures
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                              SOLUTIONS
                              • EVAPORATION/ CRYSTALLIZATION
                               • Widely differing boiling points
                               • Example: Copper sulphate + water
SUSPENSION
                              • SIMPLE DISTILLATION
                                                                                COLLOIDS
• DECANTATION.
• Different particle size.      • Widely differing boiling points               • CHROMATOGRAPHY
  • Example – chalk + water                                                       • Differing solubilities in a
                                                                                    particular solvent leading
                                                                                    to differing speeds of
• FILTRATION.                                                                       movement on
• Different particle sizes.                                                         chromatogram
                                                                                  • Example: screened methyl
                                                                                    orange




                                            Solid +
                                             Liquid
                                            mixtures
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                                                                                  Solvent extraction
                                                          Are the components
                                                           ionic, covalent or
Determinating the correct


                                                                mixed?
                                                                                     Does on the         Yes
                                                                                     components                      Sublimation
                                                                                      sublime?

                                                          Are the components
                                                            in the mixture          Do they have         Yes         Fractional
                                                               miscible?           differing boiling
                                                                                                                     distillation
separation technique



                                                                                        points?



                                                                                    Do they have         Yes
                                   What is the state of                                                           Separating funnel
                                      matter of                                  differing densities?
                                    components in
                                       mixture?

                                                                                                                     Decantation
                                                                                  Do the components
                                                                                 have widely differing
                                                                                    particle sizes?
                                                                                                                      Filtration



                                                            Is the mixture a                                        Evaporation &
                                                          solution, suspension                                      crystallization
                                                                or colloid
                                                                                  Do the components
                                                                                 have widely differing
                                                                                   boiling points?
                            Syllabus requirement met:
                                                                                                                  Simple distillation
                            identify a method of separating
                            mixtures based on their                               Chromatography
                            composition
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Experiments demonstrating the different methods of separating
mixtures
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Experiment 1
Question:

You have a mixture of sodium chloride and
 ammonium chloride. How would you separate
 them?
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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
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 Materials:     •Glass funnel, evaporating dish, Bunsen burner, heating stand
                •10g of NH4CL & NaCl mixture




                •Place a small amount of the mixture in the evaporating dish.
                •Place glass funnel over dish.
  Method:       •Light bunsen burner until a small even flame is produced.
                •Continue heating until no more ammonium chloride is deposited on
                 the funnel.




 Results &      •White solid (ammonium chloride) will be deposited on the upper

Observations:    sides of the funnel




                •The mixture contained 2 ionic solids one of which sublimes (goes
Analysis &       from solid to gas) on heating.
                •The change is reversible so when the gaseous ammonium chloride
Conclusion:      comes into contact with the cooler surface of the glass funnel it
                 returns to the solid state.




                                                                    Sublimation
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Experiment 2
Question:

You have a mixture of sodium chloride and iodine
 crystals. How would you separate them?
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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
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                • Two (2) 100 ml beakers, glass stirring rod, evaporating dish, Bunsen
                  burner, heating stand, filter paper, funnel
 Materials:     • 10g of iodine crystals (I2) & sodium chloride (NaCl) mixture
                • 10 ml of 1,1,1-trichloroethane



                •Place 10g of the mixture in beaker.
                •Add 10ml of 1,1,1-trichloroethane to beaker.
                •Stir with glass stirring rod until all iodine crystals are dissolve
  Method:       •Fold filter paper into glass funnel. Filter beaker with NaCl, I2 and solvent mixture
                 into second beaker.
                •Light Bunsen burner until a small even flame is produced.
                •Heat second beaker with I2/solvent solution until all solvent evaporates.
                •Allow residue to cool


                •On adding the 1,1,1-trichloroethane, the mixture separates into two layers.
 Results &      •The top layer is brown in colour. This contains iodine in solution.
                •The second layer is a suspension of NaCl in solvent.
Observations:   •White crystals are left as filtered residue in filter paper. The filtrate is a brown solution
                •On heating, and crystallization, brown crystals are left




Analysis &      •The mixture contained one ionic compound (NaCl) which dissolves only in polar solvents such
                 as water and one molecular compound (i2) which only dissolves in organic solvents.

Conclusion:     •The 2 components could therefore be separated by dissolving the molecular compound in the
                 organic solvent, filtering off the ionic compound and recrystallizing the molecular compound.




                                 Solvent extraction
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                                                                                  Sodium chloride (NaCl)
                                                                                   is ionic and therefore
                                                                                   only dissolves in polar


Solvent extraction
                                                                                          solvents
                                                                                                                   Sodium chloride
                                                                                                                      (NaCl (s))

                                                           Iodine (I2) is a covalent
                                                          compound and therefore
                                                        dissolves in organic solvents

                        Add 1,1,1-                                   Filter off
     Mixture of         trichloroethane        Iodine solution       NaCl (s)
       iodine +         (organic solvent)
   sodium chloride
                                              sodium chloride                                  Iodine & solvent
                                                                                                    filtrate


                                                                                                    Evaporate
                                                                                                    the
                                                                                                    solvent
                                                                                                    through
                                                                                                    slow
                                                                                                    heating
Syllabus objective                           Iodine
                                            crystals             Cool &
met:
                                                                 crystallize
identify other
methods of separation
such as solvent
extraction
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Experiment 3
Question:

You have a solution of copper (II) sulphate and
 water. How would you separate them?
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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
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      Materials:
                                            •Round bottom flask, thermometer, Bunsen burner, heating stand, Leibig
                                             condenser, Erlynmeyer flask
                                            •10ml of copper (II) sulphate solution - Cu(SO4) (aq)




                                            •Place 10 ml of CuSO4 (aq) into round-bottom flask.


        Method:
                                            •Set up the equipment as shown in diagram
                                            •Light Bunsen burner until it achieves a steady blue flame.
                                            •Heat solution steadily until the temperature reaches just above 100 °C.
                                            •Continue to heat until all the solution turns to blue crystals.




  Results &                                 •The volume of the solution decreases and changes state (from liquid to solid blue crystals).

 Observations:
                                            •A clear solution forms in the Erlenmeyer flask over time.




    Analysis &
                                            •The boiling point of water is 100°C while that of CuSO4 is 150°C.
                                            •By keeping the temperature just above 100°C but below 150°C, the water in the solution
                                             changes state from liquid to gas (water vapour).

    Conclusion:
                                            •The water vapour travels through the Leibig condenser which cools the temperature and
                                             causes the water to vapour to change back to its liquid state as this is a reversible change.
                                            •The CuSO4 remains in the round bottomed flask as its boiling point has not been reached.


Syllabus requirement met:
describe the separating methods of simple
distillation                                            Simple distillation
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                                               Thermometer
                                                                                                         Heating wire
                                                                                                             pad
                                                          Round bottom flask


                                                    Water out

         Bunsen                                                                         Leibig condenser
         burner




                                                                      Water in
                                                                                                             Erlynmeyer flask


                                                               Heating stand

                                                                                                              Syllabus requirement met:
                                                                                                              Draw line diagrams for simple
                                                                                                              distillation
Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/simple_distillation2.jpg
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Experiment 4
Question:

You have a solution of ethanol and water. How
 would you separate them?
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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
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                                     • Round bottom flask, thermometer, Bunsen burner, heating stand, heating
        Materials:                     pad Leibig condenser, Erlynmeyer flask, fractionating column
                                     • 20ml of ethanol and water solution (50/50 W/V)


                                     •Place 20 ml of solution into round-bottom flask.
                                     •Set up the equipment as shown in diagram

          Method:                    •Light Bunsen burner until it achieves a steady blue flame. Heat solution steadily until the
                                      temperature reaches 80°C.
                                     •Continue to heat until all there is no more increases in the volume of distillate collected in the
                                      Erlenmeyer flask



    Results &                        • The volume of the solution decreases by approximately 50%
                                     • A clear solution forms in the Erlenmeyer flask over time which is
   Observations:                       approximately 50% of the original volume.


                                     •The boiling point of water is 100°C while that of ethanol is 78.4°C.

      Analysis &
                                     •By keeping the temperature just above 78°C but below 100°C, the ethanol in the solution
                                      changes state from liquid to gas.
                                     •The ethanol vapour travels through the fractionating column, where it is repeated cooled

      Conclusion:
                                      and reheated as it falls back into the base of the column, removing impurities.
                                     •The vapour then passes through the Leibig condenser which cools the temperature and
                                      causes the water to vapour to change back to its liquid state as this is a reversible change.
                                     •The water remains in the round bottomed flask as its boiling point has not been reached.




                                     Fractional distillation
Syllabus requirement met:
describe the separating methods of
fractional distillation
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                                                                                 Heat is applied to the bottom of the
                                                                                 larger round bottom flask that holds the




                                             Fractional distillation apparatus
                                                                                 fermented mixture.

                                                                                 As the vapors rise in the fractionating
                                                                                 column, the higher boiling point water
                                                                                 condenses and falls back into the round
                                                                                 bottom flask.

                                                                                 The ethanol continues to rise slowly and
                                                                                 reaches the distillation head where a
                                                                                 thermometer registers its temperature.
                                                                                 If the temperature is kept at about 78 C,
                                                                                 by adjusting the heat, ethanol will flow
                                                                                 over to the Liebig condenser and turned
                                                                                 back into a liquid.

                                                                                 The Liebig condenser has a cold water
                                                                                 jacket wrapped around a central tube and
                                                                                 when the hot ethanol vapor comes in
                                                                                 contact with the walls of the inner tube, it
                                                                                 loses heat and returns to a liquid state.

                                                                                 The condensed ethanol drips down and is
                                                                                 collected in the smaller round bottom
                                                                                 flask.



Source: www.chemistrydaily.com/chemistry/upload/1/16/Fractional_distillation_lab_apparatus.png
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Experiment 5
Question:

You have a solution of oil and water. How would
 you separate them?
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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
54

                                                                         Prepared by JGL   8/9/2009




                                     • Separating funnel, clamp stand, Erlynmeyer flask
        Materials:                   • 20ml of oil and water mixture (50/50 W/V)

                                     •Set up the equipment as shown in diagram
                                     •Place 20 ml of solution into separating funnel
          Method:                     •Allow the mixture to settle then slowly release valve and allow the bottom
                                      layer to flow out into the flask below.
                                      •Close valve when the last drop of the bottom layer has been released into
                                      flask.


    Results &                        • The mixture separates into 2 distinct layers.
   Observations:

     Analysis &                      • Water has a higher density than oil. It therefore sinks to the bottom of the
                                       separating funnel.
                                     • The two components are highly immiscible, that is they do not mix well with
     Conclusion:                       each other and form a distinctly visible phase boundary between the two
                                       upon settling which allows the easy separation using just the human eye.




                                                  Separating funnel
Syllabus requirement met:
describe the separating methods of
layer separation
55

                                        Prepared by JGL   8/9/2009
Set up of separating funnel apparatus


                                                 Results of experiment
56

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Experiment 6
Question:

You have a mixture of sand and water. How would
 you separate them?
57

                                                                                  Prepared by JGL     8/9/2009




                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
58

                                                     Prepared by JGL   8/9/2009




                • 100ml beaker, 50 ml beaker, glass stirring rod
 Materials:     • 30ml of sand and water suspension (50/50 W/V)

                •Place mixture into 50 ml beaker
                •Allow to stand until the sand settles to bottom and the mixture looks fully
  Method:       transparent.
                •Pour the mixture slowly into the 100 ml beaker. Use the glass stirring rod to
                prevent any of the sand sediment from being poured into the beaker.


 Results &      • The mixture went from opaque to transparent with
Observations:     white sediment settling to the bottom upon standing.

                • The sand and water mixture formed a suspension. The solute, sand, could
                  not completely mix with the water, i.e. It was partially insoluble.
Analysis &      • The sand particles settled to the bottom as it was denser than water and
                  insoluble.

Conclusion:     • The separation of the two components after standing (this process is known
                  as sedimentation) can be done using just the eye as the separation is very
                  distinct. However, there is a possibility that some sand particles are left in
                  the beaker.



                                                  Decantation
59

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Decantation
Sedimentation                                          Decantation




Source: www.tutorbene.com/cms_images/decantation.bmp
60

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Experiment 7
Question:

You have a solution of table salt and water. How
 would you retrieve the salt from the solution?
61

                                                                                  Prepared by JGL     8/9/2009




                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
62

                                                    Prepared by JGL   8/9/2009




 Materials:     • Evaporating dish, heating pad, heating stand, Bunsen burner
                • 20ml of salt and water solution (50/50 W/V)

                •Place solution into evaporating dish
                •Set up apparatus as shown in diagram.

  Method:       •Light Bunsen burner and heat solution slowly, starting with a low flame and
                gradually increasing the heat.
                •Continue heating until all liquid evaporates.
                •Turn off Bunsen burner. Allow residue to cool.


 Results &      • All water evaporates.
Observations:   • The solution gradually turns to solid crystals.


                • The water in the solution reaches its boiling point and chnages state from

Analysis &
                  liquid to gas (water vapour).
                • NaCl is an ionic solid which has a very high boiling point as compared to
                  water and remains in the solid state.
Conclusion:     • This method is only useful for separating the mixture’s components when
                  the solvent (in this case water) is not to be retrieved at the end of the
                  experiment.




         Evaporation/ crystallization
63

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Evaporation and crystallization
          Salt water
           solution                                                                                            Evaporating dish




                                                                                                     Heating pad or wire gauze



                                                                                           Heating stand or
                                                                                                tripod




                                                                                                     Bunsen burner




Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/evaporation.jpg
64

                               Prepared by JGL   8/9/2009




Experiment 8
Question:

You have a solution of chalk and water. How
 would you retrieve both components of the
 mixture?
65

                                                                                  Prepared by JGL     8/9/2009




                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
66

                                                                                   Prepared by JGL   8/9/2009




            Materials:                            • Filter paper, funnel, 100 ml beaker, Erlenmeyer flask
                                                  • 30ml of chalk and water solution (50/50 W/V)

                                                  •Place mixture into 100 ml beaker
                                                  •Fold filter paper as shown in diagram below
                                                  •Place in funnel then place funnel into Erlenmeyer flask
             Method:                              •Pour mixture into funnel slowly until the entire mixture is transferred
                                                  without spilling out of funnel.
                                                  •Allow the mixture to separate out completely before removing the filter
                                                  paper.

         Results &                                • The chalk remains as residue on the filter paper
        Observations:                             • The water comes out in the Erlenmeyer flask


                                                  • The chalk and water mixture formed a suspension. The
                                                    solute, chalk, could not completely mix with the water, i.e. It was
                                                    partially insoluble.
          Analysis &                              • The chalk particles are larger than the water molecules and cannot
                                                    pass through the porous filter paper.
          Conclusion:                             • The water molecules are small enough to pas s through the filter
                                                    paper.
                                                  • This difference in particle size allows the chalk to be separated from
                                                    the water via the process of filtration.

Syllabus requirement met:
1. describe the separating methods of filtration
2. carry out filtration in the laboratory and write up notes about the
   procedure and results
3. recognize that filtration separates particle based on size
                                                                                             Filtration
67

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                                                                   Procedure for fluted filter paper
                                                                                                       This is used when you need to get
                                                                                                       faster filtration.




Source: www.theresasakno.com/popup/popup.asp?sid=D674F0CE-C7CB-4A46-94EA-1E79AD64C378&imgname=034.jpg
68

                                                                                       Prepared by JGL   8/9/2009
                              Water molecules


                                                                                                                    Beaker



                                               Filter paper
                                                                          Filter
                                                                          paper




                                                                                                                    Mixture of chalk
                                                                                                                       and water
                                                                                                                     (suspension)
                        Chalk particles


    The water molecules                                                                        Beaker
    are smaller than the                      Water
    chalk particles. They
    are small enough to
    pass through the
    pores of the filter
    paper.                                                                                                 Funnel



Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/filtration.jpg
69

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                                                                         How to filtrate a hot solution
                                                                                                          Materials required:
                                                                                                          1. Clamp stand,
                                                                                                          2. Short stem glass funnel
                                                                                                          3. Glass stirring rod
                                                                                                          4. Filter paper (fluted)
                                                                                                          5. Erlenmeyer flask
                                                                                                          6. Cloth

                                                                                                          A filtration procedure called "hot gravity
                                                                                                          filtration" is used to separate insoluble
                                                                                                          impurities from a hot solution.

                                                                                                          Hot filtrations require fluted filter paper
                                                                                                          and careful attention to the procedure to
                                                                                                          keep the apparatus warm but covered so
                                                                                                          that solvent does not evaporate




Source: www.chemistry.mcmaster.ca/~chem2o6/labmanual/expt1/exp1-f3.gif
70

                                                                          Prepared by JGL   8/9/2009




Vacuum Filtration
Vacuum filtration is used primarily to collect a
desired solid, for instance, the collection of
crystals in a recrystallization procedure.

Vacuum filtration uses either a Buchner or a
Hirsch funnel.

Vacuum filtration is faster than gravity
filtration, because the solvent or solution and air
is forced through the filter paper by the
application of reduced pressure. The reduced
pressure requires that they be carried out in
special equipment:
1. Buchner or Hirsch funnel
2. heavy-walled, side arm filtering flask
3. rubber adaptor or stopper to seal the funnel to
     the flask when under vacuum
4. vacuum source




                                                      Source: http://blog.khymos.org/wp-content/2007/09/stock-filtration.png
71

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Experiment 9
Question:

How would you separate the pigments in screened
 methyl orange?
72

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                                                                         Solvent extraction
                                                 Are the components
                                                  ionic, covalent or
                                                       mixed?
                                                                            Does on the         Yes
                                                                            components                      Sublimation
                                                                             sublime?
Determining the correct



                                                 Are the components
                                                   in the mixture          Do they have         Yes         Fractional
                                                      miscible?           differing boiling
                                                                                                            distillation
separation technique



                                                                               points?



                                                                           Do they have         Yes
                          What is the state of                                                           Separating funnel
                             matter of                                  differing densities?
                           components in
                              mixture?

                                                                                                            Decantation
                                                                         Do the components
                                                                        have widely differing
                                                                           particle sizes?
                                                                                                             Filtration



                                                   Is the mixture a                                        Evaporation &
                                                 solution, suspension                                      crystallization
                                                       or colloid
                                                                         Do the components
                                                                        have widely differing
                                                                          boiling points?
                                                                                                         Simple distillation

                                                                         Chromatography
73

                                                                       Prepared by JGL   8/9/2009




                                       • Chromatography paper,, glass rod, beaker
          Materials:                   • 5ml screened methyl orange, 50ml water


                                       •Screened methyl orange is dissolved in water and carefully spotted
                                       onto chromatography paper
                                       •Alongside it are spotted known colours on a 'start line'
                                       •The paper is carefully dipped into water, which is absorbed into the
            Method:                    paper and rises up it.
                                       •The distance moved by the solvent is marked on carefully with a pencil
                                       and the distances moved by each 'centre' of the coloured spots is also
                                       measured


                                       • Two different colours appear on the chromotogram at different points
       Results &                         on the paper.
                                       • Rf = distance moved by dissolved substance (solute) / distance moved
      Observations:                      by solvent.
                                       • The Rf value is calculated for each spot.


        Analysis &                     • Due to different solubilities and different molecular 'adhesion' some
                                         colours move more than others up the paper, so effecting the
        Conclusion:                      separation of the different coloured molecules.



Syllabus requirement met:


                                                    Chromatography
identify other methods of separation
such as chromatography
74

                                                         Prepared by JGL   8/9/2009


                                                                                              These are
                                                                                              the
                                                                                              pigments

Chromatography                                                                                present
                                                                                              in the dye

       The material to be separated e.g. a food
         dye (6) is dissolved in a solvent and
       carefully spotted onto chromatography
        paper sheet. Alongside it are spotted
        known colours on a 'start line' (1-5).


                  The paper is carefully dipped into a
               solvent, which is absorbed into the paper
               and rises up it. The solvent may be water
                or an organic liquid like an alcohol (e.g.
               ethanol) or a hydrocarbon, so-called non-
                           aqueous solvents.



          For accurate work the distance moved
           by the solvent is marked on carefully       Any colour which horizontally matches
        with a pencil and the distances moved by       another is likely to be the same molecule
        each 'centre' of the coloured spots is also    i.e. red (1 and 6),
         measured. These can be compared with          brown (3 and 6) and
             known substances BUT if so, the           blue (4 and 6) match,
        identical paper and solvent must be used       showing these three are all in the food dye (6).
75

                                        Prepared by JGL   8/9/2009




Methods used in industry for separating mixtures
76

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Chromatography
                 Calculation of Rf values

                 The distance a substance moves, compared to the distance the
                 solvent front moves is called the reference or Rf value

                 0.0<Rf<1.0 where
                 Rf = 0.0 (not moved - no good)
                 Rf = 1.0 (too soluble - no good either)

                 Rf ratio values between 0.1 and 0.9 can be useful for analysis
                 and identification.



                                 distance                      distance
                                 moved by                      moved by
                 Rf              dissolved                     solvent
                                 substance
                                 (solute)


                  Chromatography can be used to
                  separate the amino acids in proteins

                  and to separate drugs in pharmaceutical
                  laboratories
77

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                                                                            Centrifugation is a process that
                                                                            involves the use of the centrifugal force
                                                                            for the separation of mixtures, used in
                                                                            industry and in laboratory settings.

                                                                            More-dense components of the mixture




                                                         Centrifugation
                                                                            migrate away from the axis of the
                                                                            centrifuge, while less-dense components
                                                                            of the mixture migrate towards the axis.

                                                                            Increasing the effective gravitational
                                                                            force on a test tube causes the precipitate
                                                                            to gather on the bottom of the tube.

                                                                            The remaining solution is properly called
                                                                            the "supernate" .The supernate is then
                                                                            either quickly decanted from the tube
                                                                            without disturbing the precipitate, or
                                                                            withdrawn with a pipette




Source: http://www.freewebs.com/ltaing/centrifuge2.gif
78

                                                                                                 Prepared by JGL   8/9/2009




                                                                                                        Centrifugation is used to
                                                                                                        separate the components in
                                                                                                        blood




                                                                              Centrifugation of blood
                                                                                                        A centrifuge separates out blood
                                                                                                        components by their various
                                                                                                        densities.

                                                                                                        The red blood cells (RBCs) are
                                                                                                        denser and move to the bottom
                                                                                                        of the tube.

                                                                                                        The plasma fraction is the least
                                                                                                        dense and will float as the top
                                                                                                        layer.

                                                                                                        The "buffy coat" which contains
                                                                                                        the majority of platelets will be
                                                                                                        sandwiched between the plasma
                                                                                                        and above the RBCs.



Syllabus requirement met:
Name two industrial methods of separating mixtures - centrifugation used to
separate components of blood / body fluids in laboratory testing
79

                                     Prepared by JGL   8/9/2009




Fractional distillation in industry
Continuous fractionating   How it works
column
                           This is an industrial fractionating
                           column separating a feed stream into
                           one distillate fraction and one bottoms
                           fraction.

                           However, many industrial fractionating
                           columns have outlets at intervals up the
                           column so that multiple products
                           having different boiling ranges may be
                           withdrawn from a column distilling a
                           multi-component feed stream.

                           The "lightest" products with the lowest
                           boiling points exit from the top of the
                           columns and the "heaviest" products
                           with the highest boiling points exit from
                           the bottom.
80

                                                                   Prepared by JGL   8/9/2009




Fractionating columns in industry
                                                             Bubble cap trays in
 How it works
                                                             fractionating columns
Bubble-cap "trays" or "plates" are
one of the types of physical
devices which are used to provide
good contact between the up-
flowing vapour and the down-
flowing liquid inside an industrial
fractionating column

Syllabus requirements met:
Name two industrial methods of separating mixtures e.g.
fractional distillation used to obtained distilled spirits
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Separating Mixtures: Techniques and Everyday Applications

  • 1. Mixtures and their separations Janadi Gonzalez-Lord
  • 2. 2 Prepared by JGL 8/9/2009 Table of contents • Syllabus requirements • Pure and impure substances • Classification of mixtures • Separation of mixtures • Types of separation techniques • Experiments • Industrial uses • Separating mixtures in everyday life
  • 3. 3 Prepared by JGL 8/9/2009
  • 4. 4 Prepared by JGL 8/9/2009 Syllabus requirements - Mixtures a) differentiate between mixtures and compounds in terms of composition and formation b) recognize that the components of mixtures can be separated by simple means c) define the terms : miscible , immiscible , soluble , insoluble , heterogeneous , homogenous , and apply them correctly i.e. miscible refers to liquids , soluble to gases and solids d) identify mixtures as solutions , suspensions , colloids , emulsions based on the states of matter present and their solubility / miscibility e) define solute and solvent f) identify dissolving as one substance fitting in between the spaces of another substance . g) identify a method of separating mixtures based on their composition h) describe the separating methods of simple distillation , fractional distillation , filtration , layer separation i) draw line diagrams for the methods in (h)
  • 5. 5 Prepared by JGL 8/9/2009 Syllabus requirements - Mixtures j. carry out filtration and layer separation in the laboratory and write up notes about the procedure and results k. recognize that filtration separates particle based on size l. Identify sieving , sifting and straining as everyday methods of filtration m. observe the set up as a teacher demonstration the simple distillation process n. identify other methods of separation such as chromatography , centrifugation , solvent extraction o. suggest methods for separating mixtures based on the properties of their components e.g. sand and salt p. name two industrial methods of separating mixtures e.g. fractional distillation used to obtained distilled spirits , centrifugation used to separate components of blood / body fluids in laboratory testing , filtration in purification of domestic water supply
  • 6. 6 Prepared by JGL 8/9/2009
  • 7. 7 Prepared by JGL 8/9/2009 Matter can be sub-divided into PURE and IMPURE SUBSTANCES or MIXTURES. PURE substances can be sub-divided into ELEMENTS and COMPOUNDS IMPURE substances or MIXTURES can be sub-divided into HOMOGENOUS and HETEROGENOUS
  • 8. 8 Prepared by JGL 8/9/2009 Can be separated into Can be Can be separated separated into into Source: www.mghs.sa.edu.au/Internet/Faculties/Science/Year10/Pics/elementsAndCompounds.gif
  • 9. 9 Prepared by JGL 8/9/2009 Elements versus compounds An element.... A compound...... • consists of only one kind of • consists of atoms of two or atom more different elements • cannot be broken down into a bound together, simpler type of matter by • can be broken down into a either physical or chemical simpler type of matter means (elements) by chemical means • can exist as either atoms (e.g. (but not by physical means), argon) or molecules • has properties that are (e.g., nitrogen). different from its component elements, • always contains the same ratio of its component atoms
  • 10. 10 Prepared by JGL 8/9/2009 An element Consists of only one kind of atom Ar Ar can exist as either atoms (e.g. argon) or molecules (e.g., nitrogen). cannot be broken down into a simpler type of matter by either physical or chemical means N N If you try to break apart an atom or molecule, you get an ATOMIC BOMB N N
  • 11. 11 Prepared by JGL 8/9/2009 H H A compound O consists of atoms of two or more different elements bound together always contains the same ratio of its component atoms H H O Water (formula H2O) For every water molecule, there are 2 Hydrogen atoms for every 1 Oxygen H H O O H H atom O has properties that are different from its H H component elements O For example, hydrogen and oxygen are gases but water is a liquid H H O
  • 12. 12 Prepared by JGL 8/9/2009 Examples of elements and compounds Elements Compounds Source: www.physicalgeography.net/fundamentals/images/compounds_molecules.jpg
  • 13. 13 Prepared by JGL 8/9/2009 Compounds versus Mixtures A mixture.... Remember that a compound... • consists of two or more • consists of atoms of two or different elements and/or more different elements compounds physically bound together, intermingled • can be broken down into a • can be separated into its simpler type of matter components by physical (elements) by chemical means means, and (but not by physical means), • often retains many of the • has properties that are properties of its components. different from its component Syllabus requirement met: elements, differentiate between mixtures and • always contains the same ratio compounds in terms of composition and of its component atoms formation
  • 14. 14 Prepared by JGL 8/9/2009 A mixture can be... A mixture of different A mixture of different A mixture of different types of atoms and types of atoms types of molecules molecules N N N N O O H H H H Cl H
  • 15. 15 Prepared by JGL 8/9/2009 Match the following 1. Pure elements Answer: A, C, D 2. Elements made of SINGLE ATOMS Answer: A, D 3. An element made of MOLECULES Answer: C 4. Mixture of TWO elements Answer: E, F 5. Mixture of THREE elements Answer: H 6. Pure compounds Answer: G 7. Mixture of TWO compounds Answer: B
  • 16. 16 Prepared by JGL 8/9/2009
  • 17. 17 Prepared by JGL 8/9/2009 Mixtures can be...... Homogeneous Heterogeneous • The prefixes "homo"- indicate • The prefixes: "hetero"- sameness indicate difference. • A homogeneous mixture has • A heterogeneous mixture the same uniform appearance consists of visibly different and composition throughout. substances or phases. • Many homogeneous mixtures • The three phases or states of are commonly referred to as matter are gas, liquid, and solutions. solid. Syllabus requirements met: define the terms : heterogeneous , homogenous and apply them correctly
  • 18. 18 Prepared by JGL 8/9/2009 Example of homogeneous mixtures Some mixtures around us are things we don't even think of as mixtures. Vinegar is a homogeneous mixture of water and acetic acid (CH3COOH). Most commercial vinegars have an acetic acid content of about 5%. Acetic acid gives vinegar its characteristic odor.
  • 19. 19 Prepared by JGL 8/9/2009 Example of heterogeneous mixtures The combination of oil and vinegar in salad dressing is a common example of a HETEROGENEOUS mixture. Here the two layers are distinctly visible. Each layer by itself is considered a HOMOGENEOUS mixture.
  • 20. 20 Prepared by JGL 8/9/2009 Mixtures can be same phase..... Liquid + Liquid Solid + Gas + Solid Gas Mixtures
  • 21. 21 Prepared by JGL 8/9/2009 Or Mixtures can be mixed-phase Solid + Gas Solid + Liquid Liquid + Gas Mixtures
  • 22. 22 Prepared by JGL 8/9/2009 Gas + Gas • Example: Air ( Gas + Liquid N2, O2 , Ar, CO2 • Example: , other gases) Carbonated beverages (CO2 Liquid + in water) Liquid Solid + Liquid • Example: gasoline (a • Example: Sea mixture of water ( NaCl and hydrocarbon other salts in compounds) water) Solid + Solid + Gas Solid • Example: H2 in • Alloys – Homogeneous platinum or palladium mixtures of Mixtures metals • Example : brass (Cu/Zn)
  • 23. 23 Prepared by JGL 8/9/2009 Liquid + Liquid • EMULSION Solid + Liquid • Example: milk • SUSPENSION: Examples: Tomato juice, jello, blood • COLLOIDS: Example: glue, paint Solid + Solid Solid + Gas • Example : Gravel (sand, clay and small • Example: Smoke rocks) (Air and carbon particles) Heterogeneous Mixtures
  • 24. 24 Prepared by JGL 8/9/2009 Liquid-Liquid solutions Example: Example: Example: Oil and water Phenol and water Ethanol and water Partially Immiscible Miscible miscible Syllabus requirement met: define the terms : miscible , immiscible , and apply them correctly i.e. miscible refers to liquids Increasing mixability
  • 25. 25 Prepared by JGL 8/9/2009 Syllabus requirement met: identify mixtures as solutions , suspensions , colloids , emulsions Heterogeneous mixtures based on the states of matter present and their solubility / miscibility Solute does not fully dissolve in Solution <Solute particle Liquid + liquid solvent size< Suspension Will separate into Solute particles are clearly Solute particles do not immiscible liquids ONLY if visible settle out on standing no stabiliser added Solute particles settle out upon Solute particles can pass standing through filter paper Suspensions Colloids Emulsions Increasing solute particle size
  • 26. 26 Prepared by JGL 8/9/2009 Solutions Solute Solvent Solution homogeneous mixture substance in The substance which the which is being solute is dissolved dissolved Syllabus requirement met: Define solute and solvent
  • 27. 27 Prepared by JGL 8/9/2009 DECREASING SOLUBILITY
  • 28. 28 Prepared by JGL 8/9/2009 Table salt dissolving in water Dissolving. When a solute dissolves in a solvent, the particles of the solute fit in between the particles of the solvent. There is no chemical reaction. The change is reversible and the essential components of the mixture remains the same. Syllabus requirement met: Identify dissolving as one substance fitting in between the spaces of another substance .
  • 29. 29 Prepared by JGL 8/9/2009
  • 30. 30 Prepared by JGL 8/9/2009 A mixture of different Separate atoms and types of atoms and molecules molecules N N N N O O Can be separated by O O O O PHYSICAL MEANS into N N
  • 31. 31 Prepared by JGL 8/9/2009
  • 32. 32 Prepared by JGL 8/9/2009 SUBLIMATION SOLVENT • One substance EXTRACTION sublimes, the other • Differing solubilities does not in a particular solvent • Example: • Example: Iodine + Ammonium chloride sodium chloride + sodium chloride Solid + solid mixtures
  • 33. 33 Prepared by JGL 8/9/2009 FRACTIONAL SEPARATING DISTILLATION FUNNEL • Miscible • Immiscible • Slightly differing • Differing densities boiling points • Example: Oil + water • Example: Ethanol + water Liquid + liquid mixtures
  • 34. 34 Prepared by JGL 8/9/2009 SOLUTIONS • EVAPORATION/ CRYSTALLIZATION • Widely differing boiling points • Example: Copper sulphate + water SUSPENSION • SIMPLE DISTILLATION COLLOIDS • DECANTATION. • Different particle size. • Widely differing boiling points • CHROMATOGRAPHY • Example – chalk + water • Differing solubilities in a particular solvent leading to differing speeds of • FILTRATION. movement on • Different particle sizes. chromatogram • Example: screened methyl orange Solid + Liquid mixtures
  • 35. 35 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or Determinating the correct mixed? Does on the Yes components Sublimation sublime? Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Syllabus requirement met: Simple distillation identify a method of separating mixtures based on their Chromatography composition
  • 36. 36 Prepared by JGL 8/9/2009 Experiments demonstrating the different methods of separating mixtures
  • 37. 37 Prepared by JGL 8/9/2009 Experiment 1 Question: You have a mixture of sodium chloride and ammonium chloride. How would you separate them?
  • 38. 38 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 39. 39 Prepared by JGL 8/9/2009 Materials: •Glass funnel, evaporating dish, Bunsen burner, heating stand •10g of NH4CL & NaCl mixture •Place a small amount of the mixture in the evaporating dish. •Place glass funnel over dish. Method: •Light bunsen burner until a small even flame is produced. •Continue heating until no more ammonium chloride is deposited on the funnel. Results & •White solid (ammonium chloride) will be deposited on the upper Observations: sides of the funnel •The mixture contained 2 ionic solids one of which sublimes (goes Analysis & from solid to gas) on heating. •The change is reversible so when the gaseous ammonium chloride Conclusion: comes into contact with the cooler surface of the glass funnel it returns to the solid state. Sublimation
  • 40. 40 Prepared by JGL 8/9/2009 Experiment 2 Question: You have a mixture of sodium chloride and iodine crystals. How would you separate them?
  • 41. 41 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 42. 42 Prepared by JGL 8/9/2009 • Two (2) 100 ml beakers, glass stirring rod, evaporating dish, Bunsen burner, heating stand, filter paper, funnel Materials: • 10g of iodine crystals (I2) & sodium chloride (NaCl) mixture • 10 ml of 1,1,1-trichloroethane •Place 10g of the mixture in beaker. •Add 10ml of 1,1,1-trichloroethane to beaker. •Stir with glass stirring rod until all iodine crystals are dissolve Method: •Fold filter paper into glass funnel. Filter beaker with NaCl, I2 and solvent mixture into second beaker. •Light Bunsen burner until a small even flame is produced. •Heat second beaker with I2/solvent solution until all solvent evaporates. •Allow residue to cool •On adding the 1,1,1-trichloroethane, the mixture separates into two layers. Results & •The top layer is brown in colour. This contains iodine in solution. •The second layer is a suspension of NaCl in solvent. Observations: •White crystals are left as filtered residue in filter paper. The filtrate is a brown solution •On heating, and crystallization, brown crystals are left Analysis & •The mixture contained one ionic compound (NaCl) which dissolves only in polar solvents such as water and one molecular compound (i2) which only dissolves in organic solvents. Conclusion: •The 2 components could therefore be separated by dissolving the molecular compound in the organic solvent, filtering off the ionic compound and recrystallizing the molecular compound. Solvent extraction
  • 43. 43 Prepared by JGL 8/9/2009 Sodium chloride (NaCl) is ionic and therefore only dissolves in polar Solvent extraction solvents Sodium chloride (NaCl (s)) Iodine (I2) is a covalent compound and therefore dissolves in organic solvents Add 1,1,1- Filter off Mixture of trichloroethane Iodine solution NaCl (s) iodine + (organic solvent) sodium chloride sodium chloride Iodine & solvent filtrate Evaporate the solvent through slow heating Syllabus objective Iodine crystals Cool & met: crystallize identify other methods of separation such as solvent extraction
  • 44. 44 Prepared by JGL 8/9/2009 Experiment 3 Question: You have a solution of copper (II) sulphate and water. How would you separate them?
  • 45. 45 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 46. 46 Prepared by JGL 8/9/2009 Materials: •Round bottom flask, thermometer, Bunsen burner, heating stand, Leibig condenser, Erlynmeyer flask •10ml of copper (II) sulphate solution - Cu(SO4) (aq) •Place 10 ml of CuSO4 (aq) into round-bottom flask. Method: •Set up the equipment as shown in diagram •Light Bunsen burner until it achieves a steady blue flame. •Heat solution steadily until the temperature reaches just above 100 °C. •Continue to heat until all the solution turns to blue crystals. Results & •The volume of the solution decreases and changes state (from liquid to solid blue crystals). Observations: •A clear solution forms in the Erlenmeyer flask over time. Analysis & •The boiling point of water is 100°C while that of CuSO4 is 150°C. •By keeping the temperature just above 100°C but below 150°C, the water in the solution changes state from liquid to gas (water vapour). Conclusion: •The water vapour travels through the Leibig condenser which cools the temperature and causes the water to vapour to change back to its liquid state as this is a reversible change. •The CuSO4 remains in the round bottomed flask as its boiling point has not been reached. Syllabus requirement met: describe the separating methods of simple distillation Simple distillation
  • 47. 47 Prepared by JGL 8/9/2009 Thermometer Heating wire pad Round bottom flask Water out Bunsen Leibig condenser burner Water in Erlynmeyer flask Heating stand Syllabus requirement met: Draw line diagrams for simple distillation Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/simple_distillation2.jpg
  • 48. 48 Prepared by JGL 8/9/2009 Experiment 4 Question: You have a solution of ethanol and water. How would you separate them?
  • 49. 49 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 50. 50 Prepared by JGL 8/9/2009 • Round bottom flask, thermometer, Bunsen burner, heating stand, heating Materials: pad Leibig condenser, Erlynmeyer flask, fractionating column • 20ml of ethanol and water solution (50/50 W/V) •Place 20 ml of solution into round-bottom flask. •Set up the equipment as shown in diagram Method: •Light Bunsen burner until it achieves a steady blue flame. Heat solution steadily until the temperature reaches 80°C. •Continue to heat until all there is no more increases in the volume of distillate collected in the Erlenmeyer flask Results & • The volume of the solution decreases by approximately 50% • A clear solution forms in the Erlenmeyer flask over time which is Observations: approximately 50% of the original volume. •The boiling point of water is 100°C while that of ethanol is 78.4°C. Analysis & •By keeping the temperature just above 78°C but below 100°C, the ethanol in the solution changes state from liquid to gas. •The ethanol vapour travels through the fractionating column, where it is repeated cooled Conclusion: and reheated as it falls back into the base of the column, removing impurities. •The vapour then passes through the Leibig condenser which cools the temperature and causes the water to vapour to change back to its liquid state as this is a reversible change. •The water remains in the round bottomed flask as its boiling point has not been reached. Fractional distillation Syllabus requirement met: describe the separating methods of fractional distillation
  • 51. 51 Prepared by JGL 8/9/2009 Heat is applied to the bottom of the larger round bottom flask that holds the Fractional distillation apparatus fermented mixture. As the vapors rise in the fractionating column, the higher boiling point water condenses and falls back into the round bottom flask. The ethanol continues to rise slowly and reaches the distillation head where a thermometer registers its temperature. If the temperature is kept at about 78 C, by adjusting the heat, ethanol will flow over to the Liebig condenser and turned back into a liquid. The Liebig condenser has a cold water jacket wrapped around a central tube and when the hot ethanol vapor comes in contact with the walls of the inner tube, it loses heat and returns to a liquid state. The condensed ethanol drips down and is collected in the smaller round bottom flask. Source: www.chemistrydaily.com/chemistry/upload/1/16/Fractional_distillation_lab_apparatus.png
  • 52. 52 Prepared by JGL 8/9/2009 Experiment 5 Question: You have a solution of oil and water. How would you separate them?
  • 53. 53 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 54. 54 Prepared by JGL 8/9/2009 • Separating funnel, clamp stand, Erlynmeyer flask Materials: • 20ml of oil and water mixture (50/50 W/V) •Set up the equipment as shown in diagram •Place 20 ml of solution into separating funnel Method: •Allow the mixture to settle then slowly release valve and allow the bottom layer to flow out into the flask below. •Close valve when the last drop of the bottom layer has been released into flask. Results & • The mixture separates into 2 distinct layers. Observations: Analysis & • Water has a higher density than oil. It therefore sinks to the bottom of the separating funnel. • The two components are highly immiscible, that is they do not mix well with Conclusion: each other and form a distinctly visible phase boundary between the two upon settling which allows the easy separation using just the human eye. Separating funnel Syllabus requirement met: describe the separating methods of layer separation
  • 55. 55 Prepared by JGL 8/9/2009 Set up of separating funnel apparatus Results of experiment
  • 56. 56 Prepared by JGL 8/9/2009 Experiment 6 Question: You have a mixture of sand and water. How would you separate them?
  • 57. 57 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 58. 58 Prepared by JGL 8/9/2009 • 100ml beaker, 50 ml beaker, glass stirring rod Materials: • 30ml of sand and water suspension (50/50 W/V) •Place mixture into 50 ml beaker •Allow to stand until the sand settles to bottom and the mixture looks fully Method: transparent. •Pour the mixture slowly into the 100 ml beaker. Use the glass stirring rod to prevent any of the sand sediment from being poured into the beaker. Results & • The mixture went from opaque to transparent with Observations: white sediment settling to the bottom upon standing. • The sand and water mixture formed a suspension. The solute, sand, could not completely mix with the water, i.e. It was partially insoluble. Analysis & • The sand particles settled to the bottom as it was denser than water and insoluble. Conclusion: • The separation of the two components after standing (this process is known as sedimentation) can be done using just the eye as the separation is very distinct. However, there is a possibility that some sand particles are left in the beaker. Decantation
  • 59. 59 Prepared by JGL 8/9/2009 Decantation Sedimentation Decantation Source: www.tutorbene.com/cms_images/decantation.bmp
  • 60. 60 Prepared by JGL 8/9/2009 Experiment 7 Question: You have a solution of table salt and water. How would you retrieve the salt from the solution?
  • 61. 61 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 62. 62 Prepared by JGL 8/9/2009 Materials: • Evaporating dish, heating pad, heating stand, Bunsen burner • 20ml of salt and water solution (50/50 W/V) •Place solution into evaporating dish •Set up apparatus as shown in diagram. Method: •Light Bunsen burner and heat solution slowly, starting with a low flame and gradually increasing the heat. •Continue heating until all liquid evaporates. •Turn off Bunsen burner. Allow residue to cool. Results & • All water evaporates. Observations: • The solution gradually turns to solid crystals. • The water in the solution reaches its boiling point and chnages state from Analysis & liquid to gas (water vapour). • NaCl is an ionic solid which has a very high boiling point as compared to water and remains in the solid state. Conclusion: • This method is only useful for separating the mixture’s components when the solvent (in this case water) is not to be retrieved at the end of the experiment. Evaporation/ crystallization
  • 63. 63 Prepared by JGL 8/9/2009 Evaporation and crystallization Salt water solution Evaporating dish Heating pad or wire gauze Heating stand or tripod Bunsen burner Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/evaporation.jpg
  • 64. 64 Prepared by JGL 8/9/2009 Experiment 8 Question: You have a solution of chalk and water. How would you retrieve both components of the mixture?
  • 65. 65 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 66. 66 Prepared by JGL 8/9/2009 Materials: • Filter paper, funnel, 100 ml beaker, Erlenmeyer flask • 30ml of chalk and water solution (50/50 W/V) •Place mixture into 100 ml beaker •Fold filter paper as shown in diagram below •Place in funnel then place funnel into Erlenmeyer flask Method: •Pour mixture into funnel slowly until the entire mixture is transferred without spilling out of funnel. •Allow the mixture to separate out completely before removing the filter paper. Results & • The chalk remains as residue on the filter paper Observations: • The water comes out in the Erlenmeyer flask • The chalk and water mixture formed a suspension. The solute, chalk, could not completely mix with the water, i.e. It was partially insoluble. Analysis & • The chalk particles are larger than the water molecules and cannot pass through the porous filter paper. Conclusion: • The water molecules are small enough to pas s through the filter paper. • This difference in particle size allows the chalk to be separated from the water via the process of filtration. Syllabus requirement met: 1. describe the separating methods of filtration 2. carry out filtration in the laboratory and write up notes about the procedure and results 3. recognize that filtration separates particle based on size Filtration
  • 67. 67 Prepared by JGL 8/9/2009 Procedure for fluted filter paper This is used when you need to get faster filtration. Source: www.theresasakno.com/popup/popup.asp?sid=D674F0CE-C7CB-4A46-94EA-1E79AD64C378&imgname=034.jpg
  • 68. 68 Prepared by JGL 8/9/2009 Water molecules Beaker Filter paper Filter paper Mixture of chalk and water (suspension) Chalk particles The water molecules Beaker are smaller than the Water chalk particles. They are small enough to pass through the pores of the filter paper. Funnel Source: www3.moe.edu.sg/edumall/tl/digital_resources/chemistry/images/filtration.jpg
  • 69. 69 Prepared by JGL 8/9/2009 How to filtrate a hot solution Materials required: 1. Clamp stand, 2. Short stem glass funnel 3. Glass stirring rod 4. Filter paper (fluted) 5. Erlenmeyer flask 6. Cloth A filtration procedure called "hot gravity filtration" is used to separate insoluble impurities from a hot solution. Hot filtrations require fluted filter paper and careful attention to the procedure to keep the apparatus warm but covered so that solvent does not evaporate Source: www.chemistry.mcmaster.ca/~chem2o6/labmanual/expt1/exp1-f3.gif
  • 70. 70 Prepared by JGL 8/9/2009 Vacuum Filtration Vacuum filtration is used primarily to collect a desired solid, for instance, the collection of crystals in a recrystallization procedure. Vacuum filtration uses either a Buchner or a Hirsch funnel. Vacuum filtration is faster than gravity filtration, because the solvent or solution and air is forced through the filter paper by the application of reduced pressure. The reduced pressure requires that they be carried out in special equipment: 1. Buchner or Hirsch funnel 2. heavy-walled, side arm filtering flask 3. rubber adaptor or stopper to seal the funnel to the flask when under vacuum 4. vacuum source Source: http://blog.khymos.org/wp-content/2007/09/stock-filtration.png
  • 71. 71 Prepared by JGL 8/9/2009 Experiment 9 Question: How would you separate the pigments in screened methyl orange?
  • 72. 72 Prepared by JGL 8/9/2009 Solvent extraction Are the components ionic, covalent or mixed? Does on the Yes components Sublimation sublime? Determining the correct Are the components in the mixture Do they have Yes Fractional miscible? differing boiling distillation separation technique points? Do they have Yes What is the state of Separating funnel matter of differing densities? components in mixture? Decantation Do the components have widely differing particle sizes? Filtration Is the mixture a Evaporation & solution, suspension crystallization or colloid Do the components have widely differing boiling points? Simple distillation Chromatography
  • 73. 73 Prepared by JGL 8/9/2009 • Chromatography paper,, glass rod, beaker Materials: • 5ml screened methyl orange, 50ml water •Screened methyl orange is dissolved in water and carefully spotted onto chromatography paper •Alongside it are spotted known colours on a 'start line' •The paper is carefully dipped into water, which is absorbed into the Method: paper and rises up it. •The distance moved by the solvent is marked on carefully with a pencil and the distances moved by each 'centre' of the coloured spots is also measured • Two different colours appear on the chromotogram at different points Results & on the paper. • Rf = distance moved by dissolved substance (solute) / distance moved Observations: by solvent. • The Rf value is calculated for each spot. Analysis & • Due to different solubilities and different molecular 'adhesion' some colours move more than others up the paper, so effecting the Conclusion: separation of the different coloured molecules. Syllabus requirement met: Chromatography identify other methods of separation such as chromatography
  • 74. 74 Prepared by JGL 8/9/2009 These are the pigments Chromatography present in the dye The material to be separated e.g. a food dye (6) is dissolved in a solvent and carefully spotted onto chromatography paper sheet. Alongside it are spotted known colours on a 'start line' (1-5). The paper is carefully dipped into a solvent, which is absorbed into the paper and rises up it. The solvent may be water or an organic liquid like an alcohol (e.g. ethanol) or a hydrocarbon, so-called non- aqueous solvents. For accurate work the distance moved by the solvent is marked on carefully Any colour which horizontally matches with a pencil and the distances moved by another is likely to be the same molecule each 'centre' of the coloured spots is also i.e. red (1 and 6), measured. These can be compared with brown (3 and 6) and known substances BUT if so, the blue (4 and 6) match, identical paper and solvent must be used showing these three are all in the food dye (6).
  • 75. 75 Prepared by JGL 8/9/2009 Methods used in industry for separating mixtures
  • 76. 76 Prepared by JGL 8/9/2009 Chromatography Calculation of Rf values The distance a substance moves, compared to the distance the solvent front moves is called the reference or Rf value 0.0<Rf<1.0 where Rf = 0.0 (not moved - no good) Rf = 1.0 (too soluble - no good either) Rf ratio values between 0.1 and 0.9 can be useful for analysis and identification. distance distance moved by moved by Rf dissolved solvent substance (solute) Chromatography can be used to separate the amino acids in proteins and to separate drugs in pharmaceutical laboratories
  • 77. 77 Prepared by JGL 8/9/2009 Centrifugation is a process that involves the use of the centrifugal force for the separation of mixtures, used in industry and in laboratory settings. More-dense components of the mixture Centrifugation migrate away from the axis of the centrifuge, while less-dense components of the mixture migrate towards the axis. Increasing the effective gravitational force on a test tube causes the precipitate to gather on the bottom of the tube. The remaining solution is properly called the "supernate" .The supernate is then either quickly decanted from the tube without disturbing the precipitate, or withdrawn with a pipette Source: http://www.freewebs.com/ltaing/centrifuge2.gif
  • 78. 78 Prepared by JGL 8/9/2009 Centrifugation is used to separate the components in blood Centrifugation of blood A centrifuge separates out blood components by their various densities. The red blood cells (RBCs) are denser and move to the bottom of the tube. The plasma fraction is the least dense and will float as the top layer. The "buffy coat" which contains the majority of platelets will be sandwiched between the plasma and above the RBCs. Syllabus requirement met: Name two industrial methods of separating mixtures - centrifugation used to separate components of blood / body fluids in laboratory testing
  • 79. 79 Prepared by JGL 8/9/2009 Fractional distillation in industry Continuous fractionating How it works column This is an industrial fractionating column separating a feed stream into one distillate fraction and one bottoms fraction. However, many industrial fractionating columns have outlets at intervals up the column so that multiple products having different boiling ranges may be withdrawn from a column distilling a multi-component feed stream. The "lightest" products with the lowest boiling points exit from the top of the columns and the "heaviest" products with the highest boiling points exit from the bottom.
  • 80. 80 Prepared by JGL 8/9/2009 Fractionating columns in industry Bubble cap trays in How it works fractionating columns Bubble-cap "trays" or "plates" are one of the types of physical devices which are used to provide good contact between the up- flowing vapour and the down- flowing liquid inside an industrial fractionating column Syllabus requirements met: Name two industrial methods of separating mixtures e.g. fractional distillation used to obtained distilled spirits