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    Efficient Kugelrohr Distillation Cooling

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    ztmp
    Bulb-to-bulb distillation is a useful technique for small-scale purification of liquids. Traditionally, collecting bulbs were cooled with dry ice and acetone, which has drawbacks including potential ignition from sparks and contamination of distillates. To address these issues, the authors designed a new cooling system using dry ice in plastic or cardboard cylinders without acetone. The cylinders are adapted to the bulb shape with circular cuts, providing effective cooling while avoiding risks from acetone.

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    Efficient Kugelrohr Distillation Cooling

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    ztmp
    259 views1 page
    Bulb-to-bulb distillation is a useful technique for small-scale purification of liquids. Traditionally, collecting bulbs were cooled with dry ice and acetone, which has drawbacks including potential ignition from sparks and contamination of distillates. To address these issues, the authors designed a new cooling system using dry ice in plastic or cardboard cylinders without acetone. The cylinders are adapted to the bulb shape with circular cuts, providing effective cooling while avoiding risks from acetone.

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    Efficient Kugelrohr Distillation Cooling

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    Bulb-to-bulb distillation is a useful technique for small-scale purification of liquids. Traditionally, collecting bulbs were cooled with dry ice and acetone, which has drawbacks including potential ignition from sparks and contamination of distillates. To address these issues, the authors designed a new cooling system using dry ice in plastic or cardboard cylinders without acetone. The cylinders are adapted to the bulb shape with circular cuts, providing effective cooling while avoiding risks from acetone.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    259 views1 page

    Efficient Kugelrohr Distillation Cooling

    Uploaded by

    ztmp
    Bulb-to-bulb distillation is a useful technique for small-scale purification of liquids. Traditionally, collecting bulbs were cooled with dry ice and acetone, which has drawbacks including potential ignition from sparks and contamination of distillates. To address these issues, the authors designed a new cooling system using dry ice in plastic or cardboard cylinders without acetone. The cylinders are adapted to the bulb shape with circular cuts, providing effective cooling while avoiding risks from acetone.

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    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    of 1

    Lab Notes

    Effective Cooling System in Bulb-to-Bulb Distillation


    ulb-to-bulb distillation is a useful laboratory technique for the
    small-scale purification of liquid substances. In this microscale,
    short-path technique, a small quantity of material is redistilled
    using several glass bulbs connected in line. In some Kugelrohr models,
    heating is carried out by a built-in oven, and control of both temperature
    and stirring speed is performed by an integrated electronic controller.
    The flask containing the product to be distilled and the collecting bulbs
    are connected to a rotary device (Figure 1).
    Traditionally, cooling of the collecting bulbs has been carried out
    with dry ice in acetone (-78C), especially when working with low-boiling
    substances or when distilling under vacuum. This cooling technique has
    several drawbacks:
    a) Acetone is usually applied by a piece of cotton held with tweezers
    and may accidentally drip on the Kugelrohr apparatus and attack
    the plastic cover. It may also drip inside the housing, through the
    control buttons, and damage the electronic circuit boards.
    Acetone can also dissolve the plastic parts of the front panel and
    lead to the fusion of the buttons to the housing.
    b) Acetone, because of its low flash point (-18 C), could ignite if it
    contacts the electrical system since the rotor can generate
    sparks.
    c) From an operational point of view, the ground joints, which
    connect the glass bulbs, usually are not lubricated with vacuum
    grease to avoid contaminating the final distillate during its
    recovery. As a result, and even though the bulb-to-bulb seal is
    usually good, a reabsorption of acetone through the joints could
    happen principally when the distillation is carried out under
    vacuum. In this case, contamination of the distillate with acetone
    could become a problem, especially when dealing with
    low-boiling substances.
    To avoid these problems, we have designed and used extensively a
    new, safe, and simple cooling system. In this system, the distillation
    bulbs are cooled with dry ice without the use of acetone. As containers
    of solid dry ice (coolers), we use cheap and readily available plastic or
    cardboard cylindrical tubs of 4 to 5 cm in diameter and 10 cm in length
    (Figure 2a).
    To adapt the cylindrical container to the shape of the cooling bulb
    and to increase the cooling surface, it is recommended that two circular
    cuts be made on opposite sides of the bottom of the cylinder (Figure 2b).

    CO2(SOLID)
    Oven
    Rotor

    Kugelrohr

    Figure 1: Bulb-to-bulb distillation apparatus with a cooling system of


    open cylinders filled with dry ice.

    Diam = 45 cm

    Length = 10 cm

    Figure 2(a): Detail of the cylindrical dry-ice container of the cooling system.

    Diam = 45 cm

    Length = 10 cm

    ngel M. Montaa, Ph.D., and Pedro M. Grima


    Departamento de Qumica Orgnica, Universidad de Barcelona
    Mart i Franqus 1-11, 08028-Barcelona, Spain
    E-mail: [email protected]

    o you have an innovative shortcut or unique laboratory hint youd like to


    share with your fellow chemists? See the inside back cover for details.

    D
    86

    Aldrichimica ACTA

    VOL. 33, NO. 3

    2000

    Figure 2(b):
    Cross section of the cylindrical dry-ice
    container showing the circular cut made
    to adapt the cylinder to the rotating bulb.

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