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    Salt (Volhard Method)

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    fangirlton
    This document describes the Volhard method for determining the salt content of foods by analyzing for total chlorides. The key steps are: 1) The sample is digested with nitric acid and any organic matter is oxidized with potassium permanganate. 2) The dissolved chlorides are precipitated from solution as silver chloride using excess silver nitrate. 3) The excess silver ions are then backtitrated with thiocyanate ion using ferric alum as an indicator. 4) By determining the amount of excess silver ions, the amount of chloride in the original sample can be calculated as sodium chloride.

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    Salt (Volhard Method)

    Uploaded by

    fangirlton
    1K views3 pages
    This document describes the Volhard method for determining the salt content of foods by analyzing for total chlorides. The key steps are: 1) The sample is digested with nitric acid and any organic matter is oxidized with potassium permanganate. 2) The dissolved chlorides are precipitated from solution as silver chloride using excess silver nitrate. 3) The excess silver ions are then backtitrated with thiocyanate ion using ferric alum as an indicator. 4) By determining the amount of excess silver ions, the amount of chloride in the original sample can be calculated as sodium chloride.

    Original Description:

    Modified Volhard

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    This document describes the Volhard method for determining the salt content of foods by analyzing for total chlorides. The key steps are: 1) The sample is digested with nitric acid and any organic matter is oxidized with potassium permanganate. 2) The dissolved chlorides are precipitated from solution as silver chloride using excess silver nitrate. 3) The excess silver ions are then backtitrated with thiocyanate ion using ferric alum as an indicator. 4) By determining the amount of excess silver ions, the amount of chloride in the original sample can be calculated as sodium chloride.

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    1K views3 pages

    Salt (Volhard Method)

    Uploaded by

    fangirlton
    This document describes the Volhard method for determining the salt content of foods by analyzing for total chlorides. The key steps are: 1) The sample is digested with nitric acid and any organic matter is oxidized with potassium permanganate. 2) The dissolved chlorides are precipitated from solution as silver chloride using excess silver nitrate. 3) The excess silver ions are then backtitrated with thiocyanate ion using ferric alum as an indicator. 4) By determining the amount of excess silver ions, the amount of chloride in the original sample can be calculated as sodium chloride.

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    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
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    The key takeaways are that the Volhard method is used to determine the salt content of a sample by titrating chlorides with silver nitrate and back-titrating the excess silver ions with potassium thiocyanate using ferric alum as an indicator.

    The principle behind the Volhard method is that it involves digesting the sample with nitric acid and oxidizing any remaining organic matter with potassium permanganate. The dissolved chlorides in the sample are then precipitated with excess silver nitrate as silver chloride, and the excess silver ions are backtitrated with thiocyanate using ferric alum as the indicator.

    The reagents needed are silver nitrate solution, potassium thiocyanate solution, concentrated nitric acid, nitric acid (1+1), potassium permanganate solution, and ferric alum indicator. The apparatus needed are pipettes, burettes, and general laboratory glassware.

    SALT

    (Volhard Method)
    PRINCIPLE
    To determine salt, an analysis is made for total chlorides and
    the result is expressed as sodium chloride. The method involves
    the digestion of the sample with concentrated nitric acid and
    oxidation of any remaining organic matter with potassium
    permanganate. The dissolved chlorides in the sample are
    precipitated with excess silver nitrate as silver chloride, and
    the excess silver ions backtitrated with thiocyanate using ferric
    alum as the indicator. When all the excess silver ions have
    reacted with thiocyanate, any slight excess of thiocycnate will
    react with ferric alum to form a red-coloured complex (ferric
    thiocyanate) at the end-point. An excess of thiocyanate may react
    with the precipitated silver chloride, since the solubility
    product of silver thiocyanate is 0.01 that of silver chloride.
    The addition of nitrobenzene, diethyl ether or acetone overcomes
    this difficulty by coating the precipitated silver chloride and
    thereby withdrawing it from reaction with the thiocyanate
    solution. Nitrobenzene is toxic and its use is best avoided.
    APPARATUS
    1. Pipettes and burettes.
    2. Laboratory glassware.
    REAGENTS
    1. Ferric alum indicator: saturated aqueous solution of reagent
    grade ferric ammonium sulphate (I2H2O).
    2. Silver nitrate solution, 0.20 N - dissolve 17.04 g of silver
    nitrate, (previously dried at 110C) in distilled water and
    dilute to 1 litre. Standardize (using excess silver nitrate
    solution) against 0.10 N sodium chloride (5.845 g per litre).
    3. Potassium thiocyanate solution (0.100N) - dissolve 9.72 g of
    reagent grade potassium thiocyanate in distilled water, and
    dilute to one litre.
    4.
    5.
    6.
    7.

    Concentrated nitric acid.


    Nitric acid (1+1).
    Nitrobenzene.
    Potassium permanganate solution (5%).

    PROCEDURE

    Accurately weigh appropriate amount (about 2-3 g) of sample into


    a 300 ml Erlenmeyer flask. (For shrimp paste or other highly
    salted foods, weigh about 5 g into 250 ml volumetric flask and
    digest for about one hour in water bath to dissolve the salt.
    Filter through No. 1 filter paper. Take appropriate amount of
    this filtrate) (e.g. for shrimp paste, take 10 ml). Add 25 ml of
    0.100N silver nitrate solution, swirl flask until sample and
    solution are in intimate contact. Add 15 ml of concentrated
    nitric acid. (The silver nitrate solution must be added first,
    followed by the concentrated nitric acid. The order of addition
    ensures complete precipitation of the chlorides. If nitric acid
    is added first, loss of chloride by volatilization as hydrogen
    chloride could occur, since hydrogen chloride has a far greater
    vapour pressure than nitric acid.)
    Boil in a fume hood until dissolved and add potassium
    permanganate solution (5%) until colour disappears and the
    solution
    becomes
    colourless.
    (Should
    too
    much
    potassium
    permanganate be accidently added, colour removal can be effected
    by the addition of small quantities of sugar). Add about 15 to 25
    ml of distilled water, boil for 5 mins. Cool and dilute to about
    150 ml with distilled water. Add about 1 ml nitrobenzene, 2 ml of
    ferric alum indicator and shake vigorously to coagulate the
    precipitated silver chloride. Titrate the excess silver nitrate
    with 0.100 N potassium thiocyanate solution to a permanent light
    brown end-point. Carry out a blank titration containing 25.0 ml
    of 0.100N silver nitrate solution, 2 ml ferric alum indicator and
    15 ml of (1+1) nitric acid with 0.100N potassium thiocyanate.

    For highly salted foods requiring dilution, multiply the above

    calculation by 250/ml aliquot taken for analysis.


    REFERENCE
    Official Methods of Analysis of the AOAC, 1984, 32.033, and other
    references under other commodity headings.

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