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    The document provides instructions for purifying 2-methylpropan-2-ol through a multi-step process involving: 1) reacting it with hydrochloric acid, 2) separating the reaction mixture using a separating funnel, 3) distilling the organic layer to obtain the purified product. Safety precautions are emphasized given the hazardous nature of many of the chemicals involved, including working in a fume hood, adding acids gradually, and taking care when heating and pressurizing glassware.

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    Chemistry risk assestment

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    The document provides instructions for purifying 2-methylpropan-2-ol through a multi-step process involving: 1) reacting it with hydrochloric acid, 2) separating the reaction mixture using a separating funnel, 3) distilling the organic layer to obtain the purified product. Safety precautions are emphasized given the hazardous nature of many of the chemicals involved, including working in a fume hood, adding acids gradually, and taking care when heating and pressurizing glassware.

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    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
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    24 views2 pages

    Risk Assessment

    Uploaded by

    francesco
    The document provides instructions for purifying 2-methylpropan-2-ol through a multi-step process involving: 1) reacting it with hydrochloric acid, 2) separating the reaction mixture using a separating funnel, 3) distilling the organic layer to obtain the purified product. Safety precautions are emphasized given the hazardous nature of many of the chemicals involved, including working in a fume hood, adding acids gradually, and taking care when heating and pressurizing glassware.

    Copyright:

    © All Rights Reserved
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    of 2

    Part 1: Preparation

    1. Ensure that you are confident and safe in using a separating funnel for i) separation of mixtures and
    ii) shaking reaction mixtures and realising any resultant pressure
    2. Pour about 6.5 cm^3 of 2-methylpropan-2-ol into a 10 cm^3 measuring cylinder. 2-methylpropan-
    2-ol is hazardous if inhaled so work in a fume hood.
    3. Measure the mass of the measuring cylinder and contents.
    4. Pour the 2-methylpropan-2-ol into a 250 cm^3 conical flask.
    5. Measure the mass of the empty measuring cylinder and use this to record the exact mass of 2-
    methylpropan-2-ol you have put in the separating funnel.
    6. Using a 50cm3 measuring cylinder, measure about 20 cm^3 of concentrated hydrochloric acid.
    Concentrated hydrochloric acid causes burns and his vapour irritates the lungs so use gloves and
    work in a fume hood.
    7. Over a period of about 2 minutes, add the concentrated hydrochloric acid GRADUALLY to the 2-
    methylpropan-2-ol in the conical flask. The reaction is exothermic so be aware of pour it gradually.
    8. Place a mineral wood plug into the neck of the conical flask and gently swirl the mixture every few
    minutes.

    Part 2: Separation

    1. Using a funnel, pour the reaction mixture into a separating funnel. ENSURE THE TAP IS CLOSED SO
    AS NOT TO SPILL THE CONTENT.
    2. Allow the separating funnel to stand until the two layers have separed.
    3. Open the tap and run the lower aqueous layer into a clean 100 cm^3 conical flask
    4. Slowly add 10 cm^3 of 5% sodium hydrogencarbonate solution to the organic layer in the
    separating funnel.
    5. Put the stopper in the funnel and shake the contents gently. Carefully release the pressure build up
    in the separating funnel.
    6. Shake the contents more vigorously and again release the pressure. MAKE SURE THE FUNNEL IS
    CLOSED.
    7. Allow the two layers to separete, then remove the stopper and run off the lower aqueous layer as
    in step 2 of part 2.
    8. Repeat steps 3-7 until no more gas is given off.
    9. Add 10 cm^3 of distilled water to the separating funnel and shake again.
    10. Allow the layers to separete and then run off the lower aqueous layer – you can discard this layer.
    11. Allow the organic layer to run into a clean 100 cm^3 conical flask. This liquid contains the product
    of the reaction.
    12. Anhydrous sodium sulfate acts as a drying agent to remove any traces of water. Add small
    quantities (½ spatula measures at the time) to the organic liquid. Swirl between each addition to
    the flask until the liquid is completely clear and the soduim sulfate no longer forms clumps.

    Part 3: Distillation

    1. Set up the distillation apparatus as shown


    2. Measure the mass of a clean, dry sample tube and lid.
    3. Decant the impure organic product to the pear-shaped flask and add a few anti-bumping
    granules.
    4. Heat the liquid in the pear shaped flask gently with a small Bunsen Burner or spirit burner.
    DON’T OVERHEAT THE FLASK SO AS NOT TO MAKE IT MELT OR EXPLODE. Use a small beaker to
    receive any liquid impurities which distill over.
    5. When the temperature is close to 48°, use the sample tube to collecti the liquid. The boiling
    point of the product is 51°.
    6. When the temperature rises above 53° (or there is no more liquid in the pear shaped flask),
    stop the distillation.
    7. Put the lid on the sample tube and weigh it to find the mass of the product collected.
    8. Test a few drops of the product with a few drops of 0.4 mol dm^-3 HNO3(aq) and a few drops
    of 0.05 mol dm^-3 AgNO3(aq). HNO3 AND AgNO3 ARE HAZARDOUS AS WRITTEN IN THE
    CHART. THE PRODUCT IS DANGEROUS TO TOUCH WITHOUT GLOVES AND IT COULD BE
    CARCINOGENIC.

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