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    Experiment 4

    Uploaded by

    William Allan Arcilla
    Recrystallization is a technique used to purify organic compounds that are not obtained pure directly from a reaction. Key steps include dissolving the impure material in a hot solvent, filtering to remove insoluble impurities, allowing the solution to cool so the pure compound crystallizes out, filtering the crystals, and drying them. A good solvent dissolves the compound at high temperatures but not at low temperatures, and readily dissolves impurities. Water is suitable for recrystallizing acetanilide because it dissolves it readily at high temperatures but acetanilide is not very soluble in cold water. Fluted filter paper increases filtration speed by creating channels for solvent to flow through.

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    Experiment 4

    Uploaded by

    William Allan Arcilla
    4K views20 pages
    Recrystallization is a technique used to purify organic compounds that are not obtained pure directly from a reaction. Key steps include dissolving the impure material in a hot solvent, filtering to remove insoluble impurities, allowing the solution to cool so the pure compound crystallizes out, filtering the crystals, and drying them. A good solvent dissolves the compound at high temperatures but not at low temperatures, and readily dissolves impurities. Water is suitable for recrystallizing acetanilide because it dissolves it readily at high temperatures but acetanilide is not very soluble in cold water. Fluted filter paper increases filtration speed by creating channels for solvent to flow through.

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    Recrystallization is a technique used to purify organic compounds that are not obtained pure directly from a reaction. Key steps include dissolving the impure material in a hot solvent, filtering to remove insoluble impurities, allowing the solution to cool so the pure compound crystallizes out, filtering the crystals, and drying them. A good solvent dissolves the compound at high temperatures but not at low temperatures, and readily dissolves impurities. Water is suitable for recrystallizing acetanilide because it dissolves it readily at high temperatures but acetanilide is not very soluble in cold water. Fluted filter paper increases filtration speed by creating channels for solvent to flow through.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PPTX, PDF, TXT or read online from Scribd
    Download as pptx, pdf, or txt
    4K views20 pages

    Experiment 4

    Uploaded by

    William Allan Arcilla
    Recrystallization is a technique used to purify organic compounds that are not obtained pure directly from a reaction. Key steps include dissolving the impure material in a hot solvent, filtering to remove insoluble impurities, allowing the solution to cool so the pure compound crystallizes out, filtering the crystals, and drying them. A good solvent dissolves the compound at high temperatures but not at low temperatures, and readily dissolves impurities. Water is suitable for recrystallizing acetanilide because it dissolves it readily at high temperatures but acetanilide is not very soluble in cold water. Fluted filter paper increases filtration speed by creating channels for solvent to flow through.

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    Recrystallization

    Introduction
    Products from an organic reaction are seldom

    obtained in pure state directly from the reaction mixture. Most organic compounds are more soluble in hot solvents. Impurities present will have different solubilities from those of the desired compounds. Solvent must be properly selected.

    1. Steps in recrystallization of organic compounds


    Dissolve the impure material in a minimum amount of

    solvent Filter the hot solution Allow the substance to cool and deposit the crystals of the compound Filter the compounds from the solution Wash the crystals with a little cold solvent Dry the crystals

    2. Properties of a solvent to be well suited for recrystallizing


    Dissolve a moderate quantity of the substance to be

    purified at elevated temperature Not react with the substance to be purified Dissolve impurities readily at low temperature or not dissolve them at all Be readily removable from the purified product Inexpensive

    3. Solubility of acetanilide in hot and cold water. Why is water a good solvent for recrystallization of acetanilide?

    HOT WATER
    5.5g/ 100 mL @ 100 degrees

    COLD WATER
    0.53g/ 100 mL @ 0 degrees

    Water is a good solvent for recrystallization of acetanilide because at high temps, acetinalide dissolves in water readily but is not very soluble at low temps.

    4.Why is fluted paper used in the filtration process?


    A fluted filter paper is used to increase the surface area

    of the filter paper and make the filtration more efficient.

    The fluting creates gaps between the filter paper and the funnel in which it is resting. These gaps provide channels for the solvent to flow through after it passes through the filter paper, thus greatly increasing the speed of solvent flow through the paper.

    Objectives
    To be able to purify the crude sample through

    recrystallization

    Procedure:
    Weigh about 1.0g sample in a 100mL beaker and pour 25mL

    of water. Then heat the contents with stirring.

    When residue has gone into solution, remove the flame

    and add about 0.5g of charcoal.

    Continue heating with vigorous stirring and bring the

    solution to a boil.

    Then filter through a hot stemless funnel fitted with a

    fluted filter paper without delay.

    Divide the filtrate to two equal amounts in separate 50mL

    beaker. Cover one beaker with watch glass and set it aside to cool slowly.

    Place other beaker in an ice water mixture and stir rapidly while cooling.

    Data
    Weight of container 52.03g Weight of filter paper Weight of filter paper + crystallized sample Weight of crystallized sample 0.75g 1.15g

    Weight of 53.03g container + sample

    Weight of sample

    1g

    0.40

    Percentage yield of purified crystals:

    %yield = weight of pure product x 100 weight of crude sample = 0.4g x 100 1g = 40%

    Observations
    Pinkish color diminished as charcoal was added
    Smaller crystals are formed in rapid recrystallization

    process than slow recrystallization process Faster crystallization in low temperature.

    1.) Why must the hot solution be filtered without delay?


    Hot solution must be filtered without delay because if

    there is delay, the temperature would drop. This will allow crystallization of the organic content in the hot solution. Crystals would then be filtered with the impurities present.

    2.) If charcoal and sugar were the main impurities present in the crude sample, would recrystallization from water be a good method of purification? Why?
    If charcoal and sugar were the main impurities

    present, water would be a good method of purification. Charcoal can be filtered easily since it is not soluble with water. Thus, it is now separated from sugar and the organic content. When the pure sample crystallizes, sugar would still be left dissolved in water.

    3. Why can water-ethanol but not water-hexane be used as a solvent?


    Water-ethanol can be used as a solvent because water

    and ethanol are both polar substances water-hexane one is polar and the other is nonpolar.

    4. How do you account for the formation of crystals different sizes in slow and rapid crystallizing process?
    In rapid crystallizing process- the crystals are smaller

    and finer. It is because of the stirring, the particles are not compact. The time it took for the crystals to crystallize was short because of the temperature.
    In slow crystallizing process- the crystals are greater in

    terms of size because they are undisturbed.

    5. List the chief reasons why a process of crystallization would not give a yield of 100%?
    There is always some dissolved chemical left in the solution, even in small amounts
    Transferring of crystals on different containers

    may lessen the amount Some may evaporate

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