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    Moisture Determination

    Uploaded by

    Samuel Pelayo
    Here are the steps to solve the problem: a. To determine the water equivalence factor (F): F = 0.1566 x W / V = 0.1566 x 235 mg / 7.46 ml = 5.841 mg/ml b. To compute for % water: % Water = (Volume of titrant x F) x 100 / Weight of sample = (20 ml x 5.841 mg/ml) x 100 / 3.65 g = 2.43% Therefore, the % water content of the given sodium citrate sample is 2.43%

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    Moisture Determination

    Uploaded by

    Samuel Pelayo
    416 views3 pages
    Here are the steps to solve the problem: a. To determine the water equivalence factor (F): F = 0.1566 x W / V = 0.1566 x 235 mg / 7.46 ml = 5.841 mg/ml b. To compute for % water: % Water = (Volume of titrant x F) x 100 / Weight of sample = (20 ml x 5.841 mg/ml) x 100 / 3.65 g = 2.43% Therefore, the % water content of the given sodium citrate sample is 2.43%

    Original Description:

    Moist

    Original Title

    MOISTURE-DETERMINATION

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    Here are the steps to solve the problem: a. To determine the water equivalence factor (F): F = 0.1566 x W / V = 0.1566 x 235 mg / 7.46 ml = 5.841 mg/ml b. To compute for % water: % Water = (Volume of titrant x F) x 100 / Weight of sample = (20 ml x 5.841 mg/ml) x 100 / 3.65 g = 2.43% Therefore, the % water content of the given sodium citrate sample is 2.43%

    Copyright:

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

    Moisture Determination

    Uploaded by

    Samuel Pelayo
    Here are the steps to solve the problem: a. To determine the water equivalence factor (F): F = 0.1566 x W / V = 0.1566 x 235 mg / 7.46 ml = 5.841 mg/ml b. To compute for % water: % Water = (Volume of titrant x F) x 100 / Weight of sample = (20 ml x 5.841 mg/ml) x 100 / 3.65 g = 2.43% Therefore, the % water content of the given sodium citrate sample is 2.43%

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    of 3

    MOISTURE DETERMINATION

     Official Drugs vary in their water content.


     Water available either as water of crystallization (hydrates) or as water in the adsorbed form.
     Determination of this constant is necessary to specify certain water content limits in the drug
    monographs.

    Water Content is determined by any one of the SIX METHODS

    1. Gravimetric Method – for drugs containing no constituents other than water, volatile at 105C.
    2. Gravimetric Method – for drugs containing ether-soluble constituents, volatile at 105C.
    3. Azeotropic Method or toluene distillation - for the determination of moisture content of many
    vegetable drugs containing 2% or more of moisture
    4. Titrimetric Method or Karl Fischer Method - for crystalline compounds that contain water of hydration
    or absorbed water
    5. Dew Point Method – for determining Water at Very Low Concentration
    6. Electrolytic Hygrometric – for determining Extremely Low Concentration of Water

    WATER CONTENT DETERMINATION OFFICIAL METHODS

    METHOD I. Titrimetric Method/ Karl-Fischer Method


    Ia – direct Titration
    Ib – Residual titration
    Ic - Coulomteric titration
    “1 mL of the reagent is equivalent to approximately 5 milligrams of water”

    • This method is the most rapid, requires only a small sample and is specific for water.
    • The method involves titration of the sample in reagent methanol with Karl Fischer reagent, which
    consists of iodine, sulfur dioxide, pyridine, and methanol.
    • The Karl Fischer reagent has a concentration such that one mL of the reagent is equivalent to
    approximately five milligrams of water. (1 ml = 5 mg of water)
    • The reagent deteriorates gradually; it is standardized by employing sodium tartrate (Na2C4H4O6.2H2O)
    as a primary standard.

    • The water equivalence (F) mg of water per mL of the reagent is given by the formula

    0.1566 X W
    V
    • Where W is the weight in mg of sodium tartrate and V is the volume in mL of the reagent required.

    • Percent Water Content is given by the formula

    BR x F
    %Water Content = x 100
    Wt
    • Where BR (Volume of Reagent used), F (Water Equivalence) and Wt (Weight of sample)
    Practice Problem

    1. Moisture content of citric acid was determined by the Karl-fischer Method and the following data were
    obtained
    wt of citric acid …………………………4.8 g
    vol of reagent used ……………………20 ml
    Water equivalence factor of the reagent was determined by titrating 0.350 g of sodium tartrate with 10 ml
    of KFR, determine the water content of citric acid
    0.1566 x W
    F=
    V
    0.1566 x 350 mg
    F=
    10 mL
    F=5.841

    BR x F
    %Water Content= x 10 0
    Wt
    20 mL x 5.841
    %Water Content= x 10 0
    4800 mg
    % Water Content = 2.43%

    METHOD II. Azeotropic Method/ Distillation Method


    • The Azeotropic Method is specified for the determination of moisture content of many vegetable drugs
    containing 2% or more of moisture.
    • Its disadvantage is the need for a large amount of drug, from fifty (50) to one hundred (100) grams
    must be used in order to secure a volume of water that can be measured conveniently without
    considerable error.

    METHOD III. Gravimetric Method/ Drying/Thermal Method


    Method of choice for chemical samples (1-2 grams), vegetable drugs and biologics
    • When the drug contains matter other than water which is volatile at 105C, the volatile ether soluble
    extractive must be determined and the weight of this extractive is subtracted from the weight less by
    the drug upon drying, the difference is the moisture content of the drug.

    Online Assessment: (Email your assessment at [email protected], for questions/inquiries please free to
    message in this Group chat)

    1. From the assay of sodium citrate sample using Karl Fischer method, the following results were obtained:
    Wt of sample 3.65 g sample
    Vol of titrant 20 ml
    Wt of primary standard 235 mg
    Vol consumed during titration 7.46 ml
    a. Determine the water equivalence factor
    b. Compute for % water

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