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    Draft East African Standard: DEAS 847-5: 2015

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    Adufe Rufai

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    Draft East African Standard: DEAS 847-5: 2015

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    DEAS_847-_5-_Determination_of_unsaponifiable_matter

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    Draft East African Standard: DEAS 847-5: 2015

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    Adufe Rufai

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    DEAS 847-5: 2015

    ICS 71.100.70

    DRAFT EAST AFRICAN STANDARD

    Oils for cosmetic industry — Methods of test

    Part 5: Determination of unsaponifiable matter

    EAST AFRICAN COMMUNITY

    © EAS 2015 First Edition 2015


    DEAS 847- 5: 2015
    Copyright notice
    This EAC document is copyright-protected by EAC. While the reproduction of this document by
    participants in the EAC standards development process is permitted without prior permission from
    EAC, neither this document nor any extract from it may be reproduced, stored or transmitted in any
    form for any other purpose without prior written permission from EAC.

    Requests for permission to reproduce this document for the purpose of selling it should be addressed
    as shown below or to EAC’s member body in the country of the requester:

    © East African Community 2014 — All rights reserved


    East African Community
    P.O.Box 1096
    Arusha
    Tanzania
    Tel: 255 27 2504253/8
    Fax: 255 27 2504481/2504255
    E-mail: eac@eachq.org
    Web: www.eac-quality.net

    Reproduction for sales purposes may be subject to royalty payments or a licensing agreement.
    Violators may be persecuted

    ©EAC 2005– All rights reserved 1


    DEAS 847- 5: 2015
    Foreword

    Development of the East African Standards has been necessitated by the need for harmonizing
    requirements governing quality of products and services in the East African Community. It is envisaged that
    through harmonized standardization, trade barriers that are encountered when goods and services are
    exchanged within the Community will be removed.

    In order to achieve this objective, the Community established an East African Standards Committee
    mandated to develop and issue East African Standards.

    The Committee is composed of representatives of the National Standards Bodies in Partner States, together
    with the representatives from the private sectors and consumer organizations. Draft East African Standards
    are circulated to stakeholders through the National Standards Bodies in the Partner States. The comments
    received are discussed and incorporated before finalization of standards, in accordance with the procedures
    of the Community.

    East African Standards are subject to review, to keep pace with technological advances. Users of the East
    African Standards are therefore expected to ensure that they always have the latest versions of the
    standards they are implementing.

    DEAS 847-5 was prepared by Technical Committee EAS/TC 071, Cosmetics and cosmetic products.
    DEAS 847- 5: 2015

    Oils for cosmetic industry — Methods of test

    Part 5: Determination of unsaponifiable matter

    1. Scope

    This Standard gives the test method for the determination of unsaponifiable matter in oils for cosmetic
    industry

    2. Principle

    The material is completely saponified with alcoholic potassium hydroxide solution and extracted with
    petroleum ether. The petroleum ether extract is washed with aqueous alcohol and then again with water.
    The washed ether extract is evaporated and the residue weighed. Unsaponifiable matter is this residue
    minus the fatty acid present in it, which is determined by titration with sodium hydroxide solution in alcoholic
    medium.

    3. Apparatus

    3.1 Flat-bottomed or Conical Flask - 250 to 300 ml capacity. An ordinary round, flat-bottomed flask fitted
    with a long glass tube which acts as a condenser, may also be used.

    3.2 Separating Funnels - 500 ml capacity.

    4. Reagents

    4.1 Alcoholic Potassium Hydroxide Solution - Dissolve 70 to 80 g of potassium hydroxide in an equal


    quantity of distilled water, and add aldehyde-free ethyl alcohol (95 percent by volume) or aldehyde-free
    rectified spirit to make up to 1000 ml. Allow to stand overnight, decant the clear liquid and keep in a
    bottle closed tightly with a cork or rubber stopper.

    4.2 Ethyl Alcohol - aldehyde-free ethyl alcohol (95 percent by volume) or Absolute ethanol or rectified
    spirit.

    4.3 Phenolphthalein Indicator Solution - Dissolve one gram of phenolphthalein in 100 ml of ethyl alcohol.

    4.4 Petroleum Ether - Analytical Grade 40-60ºC

    4.5 Aqueous Alcohol - containing 10 percent (by volume) of ethyl alcohol.

    4.6 Standard Sodium Hydroxide Solution - approximately 0.02N.

    4.7 Acetone - Free from evaporation residue.

    5. Procedure

    Weigh accurately about 5 g of the well-mixed sample into the flask. Add 50 ml of alcoholic potassium
    hydroxide solution (see 4.1). Boil gently but steadily under a reflux condenser for one hour or until the
    saponification is complete. Wash the condenser with about 10 ml of ethyl alcohol, cool the mixture and
    transfer it to a separating funnel. Complete the transfer by washing the flask first with some ethyl alcohol and
    then wash with cold water. Altogether, add 50 ml of water to the separating funnel followed by an addition of
    50 ml of petroleum ether.
    DEAS 847- 5: 2015

    5.2 Insert the stopper and shake vigorously for at least one minute, releasing the pressure at intervals,
    and allow to settle until both the layers are clear. Transfer the lower layer containing the soap solution
    to another separating funnel, and repeat the ether extraction at least six times more using 50 ml of
    petroleum ether for each extraction. If any emulsion is formed, add a small quantity of ethyl alcohol or
    alcoholic potassium hydroxide solution.

    5.3 Collect all the ether extracts in a separating funnel. Wash the combined extracts in the funnel three
    times with 25 ml portions of aqueous alcohol shaking vigorously and drawing off the alcohol-water
    layer after each washing. Again wash the ether layer successively with 20 ml portions of water until
    the wash-water no longer turns pink on addition of a few drops of phenolphthalein indicator solution.
    Do not remove any of the ether layers. Transfer the ether layer to a tared flask containing a few
    pieces of pumice stone, and evaporate to dryness on a water-bath r. To remove the last traces of
    o
    ether and water, place the flask in an air-oven at 105 C for about one hour.

    5.4 Cool in a desiccator and weigh. Repeat the evaporation, cooling and weighing until a constant weight
    is obtained.

    5.5 After weighing, take up the residue in 50 ml of warm neutral ethyl alcohol, containing a few drops of
    phenolphthalein indicator solution and titrate with standard sodium hydroxide solution.

    6. Calculation

    6.1 Weight (B) in g of the fatty acids in the extract (as oleic acid)

    B = 0.282 VN

    where,

    V = volume in ml of standard sodium hydroxide solution, and


    N = normality of standard sodium hydroxide solution

    6.2 Unsaponifiable matter, per cent by mass

    = 100 (A – B)
    m

    where,

    A = mass in g of the residue (see 5.3)


    B = mass in g of the fatty acids in the extract (see 6.1) and
    m = mass in g of the material taken for the test

    © EAC 2015 – All rights reserved

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