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    Limit Test of Arsenic and Lead: - Tashi (91901263048)

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    Tshering Yangzom Namda
    1) Limit tests are qualitative or semi-quantitative tests used to detect small amounts of impurities commonly found in pharmaceutical substances. They work by comparing the color or turbidity produced in a sample to that of a standard. 2) The limit test for arsenic uses a Gutzeit apparatus, which reduces arsenic in a sample to arsine gas. This gas reacts with mercuric chloride paper, producing a yellow stain whose intensity depends on the arsenic content. 3) The limit test for lead uses dithizone, which forms a red complex with lead in an alkaline medium. The color produced in the sample is compared to a standard to determine if the lead content passes the

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    Limit Test of Arsenic and Lead: - Tashi (91901263048)

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    Tshering Yangzom Namda
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    1) Limit tests are qualitative or semi-quantitative tests used to detect small amounts of impurities commonly found in pharmaceutical substances. They work by comparing the color or turbidity produced in a sample to that of a standard. 2) The limit test for arsenic uses a Gutzeit apparatus, which reduces arsenic in a sample to arsine gas. This gas reacts with mercuric chloride paper, producing a yellow stain whose intensity depends on the arsenic content. 3) The limit test for lead uses dithizone, which forms a red complex with lead in an alkaline medium. The color produced in the sample is compared to a standard to determine if the lead content passes the

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    1) Limit tests are qualitative or semi-quantitative tests used to detect small amounts of impurities commonly found in pharmaceutical substances. They work by comparing the color or turbidity produced in a sample to that of a standard. 2) The limit test for arsenic uses a Gutzeit apparatus, which reduces arsenic in a sample to arsine gas. This gas reacts with mercuric chloride paper, producing a yellow stain whose intensity depends on the arsenic content. 3) The limit test for lead uses dithizone, which forms a red complex with lead in an alkaline medium. The color produced in the sample is compared to a standard to determine if the lead content passes the

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    120 views17 pages

    Limit Test of Arsenic and Lead: - Tashi (91901263048)

    Uploaded by

    Tshering Yangzom Namda
    1) Limit tests are qualitative or semi-quantitative tests used to detect small amounts of impurities commonly found in pharmaceutical substances. They work by comparing the color or turbidity produced in a sample to that of a standard. 2) The limit test for arsenic uses a Gutzeit apparatus, which reduces arsenic in a sample to arsine gas. This gas reacts with mercuric chloride paper, producing a yellow stain whose intensity depends on the arsenic content. 3) The limit test for lead uses dithizone, which forms a red complex with lead in an alkaline medium. The color produced in the sample is compared to a standard to determine if the lead content passes the

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    Limit Test of Arsenic and

    Lead
    - Tashi (91901263048)
    What is a limit test?
    These are qualitative or semi- quantitative
    tests designed to detect and limit small
    quantities of impurities that are commonly
    present in pharmaceutical substances.
    They are based on the comparison of
    opalescence, turbidity or color produced
    due to impurity in a sample with that
    produced in a standard under the same
    test conditions.
    2
    Limit test for
    Arsenic

    3
    Principle;
    Limit test of Arsenic is based
    on the reaction between arsine
    gas with hydrogen ion to form
    yellow stain on mercuric
    chloride paper in the presence
    of reducing agents like
    potassium iodide.

    4
    Requirements ;
    Arsenic apparatus,
     lead acetate solution,
    Mercuric chloride paper,
    1 M potassium iodide solution,
    Zinc dust (As T), water bath, arsenic standard
    solution (10 ppm As),
    1 ml bulb pipette, 5 ml pipette,
    Stannated hydrochloric acid
    Together, it is called Gutzeit apparatus and so the
    limit test for arsenic is also called Gutzeit test.
    5
    Gutzeit
    Gutzeit pparag
    apparatus
    6
    Working:
    Arsenic, present as arsenic acid (H3AsO4) in the sample is
    reduced to arsenious acid (H3AsO3) by reducing agents like
    potassium iodide, stannous acid, zinc, hydrochloric acid.
    sample + dil. HCL  H3AsO4(arsenic acid)
    H3AsO4 + H2SnO2(stannic acid)  H3AsO3 + H2SnO3 (stannic
    oxide)

    Arsenious acid is further reduced to arsine (gas) (AsH3) by


    the action of nascent hydrogen which is produced by
    reaction between zinc and HCL.
    H3AsO3 + 6[H]  AsH3 (arsine) + 3H2O

    The liberated arsine gas reacts with mercuric chloride paper


    to give yellow stain. 7
    Procedure for preparation of test and standard
    solutions:
    Test sample Standard solution

    Dissolve specific amount of sample in Keep a known quantity of dilute arsenic


    water and arsenic free stannated HCl solution in water and arsenic free
    and keep in a wide-mouthed bottle. stannated HCl in a wide-mouthed bottle

    Add 1 gm of potassium iodide (KI) Add 1 gm of potassium iodide (KI)

    Add 5 ml stannous chloride acid solution Add 5 ml stannous chloride acid solution

    Add 10 gm of granulated zinc and keep Add 10 gm zinc and keep the solution
    the solution aside for 40 mins aside for 40 mins

    Compare the stains obtained on both the mercuric chloride papers (The depth of
    yellow stain on the mercuric chloride paper will depend on the quantity of arsenic
    impurity present in the substance)

    8
    Inference :
    If the stain/ color intensity observed in the
    test solution is less than the standard
    solution, the sample is to have passed the
    limit test and vice-versa.

    9
    Limit test
    for Lead

    10
    Principle ;
    The limit test for lead is based on
    the reaction between lead and
    diphenylthiocarbazone
    (dithizone) in an alkaline medium
    to form lead-dithizone complex
    which is red in color.
    Dithizone is green in color in chloroform and
    lead-dithizone complex is violet in color, so the
    resulting color at the end of the process is red.
    11
    Working ;

    12
    Apparatus used: Separating funnel

    13
    Procedure
    Test Sample Standard Solution

    A known quantity of it is taken in a A standard lead solution is prepared


    separating funnel. equivalent to the amount of lead permitted
    in the sample under examination.

    Add 6ml ammonium citrate. Add 6ml ammonium citrate.

    Add 2ml potassium cyanide and 2ml Add 2ml potassium cyanide and 2ml
    hydroxylamine hydrochloride. hydroxylamine hydrochloride.

    Add two drops of phenol red. Add two drops of phenol red.

    Make the solution alkaline by adding Make the solution alkaline by adding
    ammonia solution. ammonia solution.

    Extract 5ml dithizone and mix until it Extract 5ml dithizone and mix until it
    becomes green. becomes green.
    14
    Test Sample Standard Solution
    Combine the solution with 30ml nitric Combine the solution with 30ml nitric
    acid and shake it for 30 mins. Discard acid and shake it for 30 mins. Discard
    the chloroform layer. the chloroform layer.

    To the acid solution, add 5ml standard To the acid solution, add 5ml standard
    dithizone solution. dithizone solution.

    Add 4ml ammonium cyanide. Add 4ml ammonium cyanide.

    Shake the mixture for 30 mins. Shake the mixture for 30 mins.

    Observe the color. Observe the color.

    Compare the intensities of the colors obtained in both the solutions.

    15
    Inference;
    The color produced in the sample
    solution should not be greater
    than the standard solution. If the
    color produced in the sample
    solution is less than the standard
    solution, the sample is to have
    passed the limit test and vice
    versa.
    16
    17

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