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    Back Titration (Indirect Titration)

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    naomi
    Back titrations involve an initial titration where an analyte reacts with excess reagent, followed by a second titration of the remaining excess reagent. This allows the amount of excess reagent used in the first titration to be determined, and thereby the concentration of the original analyte. Back titrations are used when one reactant is volatile, a reaction is too slow, or the analyte is insoluble or contains impurities that could interfere with direct titration.

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    Back Titration (Indirect Titration)

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    naomi
    290 views31 pages
    Back titrations involve an initial titration where an analyte reacts with excess reagent, followed by a second titration of the remaining excess reagent. This allows the amount of excess reagent used in the first titration to be determined, and thereby the concentration of the original analyte. Back titrations are used when one reactant is volatile, a reaction is too slow, or the analyte is insoluble or contains impurities that could interfere with direct titration.

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    Gravimetric

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    Back titrations involve an initial titration where an analyte reacts with excess reagent, followed by a second titration of the remaining excess reagent. This allows the amount of excess reagent used in the first titration to be determined, and thereby the concentration of the original analyte. Back titrations are used when one reactant is volatile, a reaction is too slow, or the analyte is insoluble or contains impurities that could interfere with direct titration.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    290 views31 pages

    Back Titration (Indirect Titration)

    Uploaded by

    naomi
    Back titrations involve an initial titration where an analyte reacts with excess reagent, followed by a second titration of the remaining excess reagent. This allows the amount of excess reagent used in the first titration to be determined, and thereby the concentration of the original analyte. Back titrations are used when one reactant is volatile, a reaction is too slow, or the analyte is insoluble or contains impurities that could interfere with direct titration.

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    © All Rights Reserved
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    of 31

    Back Titration (Indirect Titration)

    • It is generally a two-stage analytical technique


    • A titration method where the concentration of an
    analyte is determined by reacting it with a known
    amount of excess reagent.
    • The remaining excess reagent is then titrated
    with another second reagent.
    • The second titration's results show how much of
    the excess reagent was used in the first titration
    and the original analyte's concentration can then
    Back Titration (Indirect Titration)
    Back titrations are used when:
    • One of the reactants is volatile, e.g. ammonia.
    • A particular reaction is too slow
    • Direct titration would involve a weak acid - weak
    base titration in which the end-point is very
    difficult to observe
    • The analyte is in solid form or an insoluble salt,
    e.g. calcium carbonate
    • The analyte may contain impurities which may
    interfere with direct titration.
    • Analytical Techniques are the methods used for the
    qualitative and quantitative determination of concentration
    of a compound by using various techniques
    • Analytical methods for rapid determination of chemicals,
    biomolecules or cells are of growing interest in various
    fields such as environmental control, drug development,
    health protection, forensics and biotechnology
    • Analytical techniques are procedures or a methods how to
    analyse
    • analytical techniques are methods used to identify, isolate
    or quantify chemicals or materials, or to characterize their
    physical properties.
    • techniques are defined as the chemical or physical
    principles employed to study a substance
    • It is the study of the separation, identification, and
    quantification of the chemical components of natural and
    Gravimetric titrimetry
    Gravimetric Titrimetry

    • The mass of the standard reagent is measured.


    • The ion being analysed is completely precipitated.
    The precipitate must be a pure compound.
    Gravimetric analysis is based on conversion of
    ions/elements/radicals into a stable and pure
    compound through precipitation, which can be
    directly weighed and quantified.
    • Eg. BaCl2 + H2SO4 BaSO4 + 2HCl
    • Filtered and dried and put in weighing crucible and
    ignited. SO4 in BaSO4 is released as SO2 gas Ba is
    left as residue.
    .
     Basics: Weight amount of Analyte solution is taken It is
    precipitated using suitable reagent Precipitate produced is a
    pure and stable compound.
     Wt. of Analyte = [Wt of precipitate x gravimetric factor]
    Wt of sample
     % of Analyte = Wt. of analyte x 100

     % A = weight of ppt x gravimetric factor (G.F.) x 100


    weight of sample •
     G.F. = FW[analyte] / FW[precipitate]

    Advantage:
     Analysis is done accurately by using sensitive and moderate
    balance. Direct measurement of the compound is done so no
    calibration is required. It is an absolute method.
    Gravimetric Analysis (GA)

     GA = Quantitative Analysis by
    weight
     GA is the process of isolating and
    weighing an element or a definite
    compound of the element in as pure
    form as possible.

     Major Types of Gravimetric


    Methods:
    1. Precipitation Method
    2. Volatilization Method
    Types of Gravimetric Methods
    Precipitation Methods:
     Analyte is converted to a sparingly soluble precipitate.
     Precipitate is → filtered → washed (to remove impurities)
    → converted to a product of known composition by suitable
    heat treatment → the product is weighed.
    Volatilization Methods:
     Analyte or its decomposition products are volatilized
    at a suitable temperature.
     The volatile product → collected → weighed or the
    mass of the product is determined indirectly from the
    loss in mass of the sample.
    Precipitation Methods

    Dissolve Sample
    ↓
    Add Precipitating Agent
    ↓
    Precipitation of Constituent
    ↓
    Separation by Filtration
    ↓
    Washing (to remove soluble
    salt)
    ↓
    Drying
    ↓
    Weighing
    Precipitation Methods: Examples

    Ex-1: Determination of lead (Pb+2)


    Pb2+ + 2Cl- → PbCl2(s)

     Mass of PbCl2 is then determined

     Calculate the amount of Pb+2 in original solution

    Ex-2: Determination of Silver


    Ag+ + Cl- (excess) → AgCl (s)
    Criteria for Successful Analysis of
    Precipitation Method

     Precipitate must be insoluble so that no appreciable


    loss occurs during washing and filtration
     Easily Filterable; particle should not pass through
    the filtering medium and should not be affected by
    washing process.
     Pure (free from impurities)

     The precipitate must be a pure substance of


    definite/known chemical composition
    Criteria for Successful Analysis of
    Precipitation Method

    Filterability:
     Particles must to be large enough to collect on filter
    Crystals
     Doesn’t clog filter

     Doesn’t pass through filter

     Best Case: Pure Crystals

     Worst Case: Colloidal/Flocculated Suspension


    Flocculated
     Difficult to filter due to small size suspension
     Tend to stay in solution indefinitely
    (suspended by Brownian motion)
     Usually 1-100 nm in size
    Colloidal
    Solution
    Criteria for Successful Analysis of
    Precipitation Method

    Precipitation Process
    Process of Crystal Growth: Two Phases
    (i) Nucleation: molecules in solution come together
    randomly and form small aggregates

    (ii) Particle growth: addition of molecules to a


    nucleus to form a crystal
    Criteria for Successful Analysis of
    Precipitation Method

    Precipitation Process
     Nucleation and particle growth always compete for
    molecules/ions being precipitated.
     If nucleation is faster than particle growth:
     a large number of small aggregates occur giving colloidal
    suspensions

     If particle growth is faster than nucleation:


     only a few, large particles form giving pure crystals

    Crystal formation
    Criteria for Successful Analysis of
    Precipitation Method

    Precipitation Process
     Rates of nucleation vs. particle growth depends on
    the amount of precipitation solute present
     Relative Supersaturation (R) R  Q  S
    S
    S = solubility of precipitate in the medium from which it is being precipitated
    Q = concentration of reactants before precipitation

     Particle Size 1/R


     When R is large, the precipitate tends to be colloidal;
     When R is small, a crystalline solid is more likely
    Criteria for Successful Analysis of
    Precipitation Method

    The optimum conditions for precipitation which make the


    supersaturation low are
    1. Increase temperature of solution
     Increases S
     Increase amount of solute that can be in solution at equilibrium
    2. Add precipitating reagent slowly with stirring
     Avoids local high concentrations of precipitant
     Avoids nucleation and colloid formation
    3. Keep volume of solution large
     Keep concentration of analyte and precipitating reagent low
    4. Control S through chemical means
     By adjusting pH
     Adding complexing agents
    Gravimetric Volatilization Method:
    Example

     Determination of the sodium hydrogen carbonate


    content of antacid tablet by a gravimetric
    H2SO4 (aq) → CO2 (g)+ H2O (l)+ NaHSO4(aq)
    NaHCO3 (aq)+method
    volatilization
    GA: Advantages

     Accurate and precise, when using modern


    analytical balances.
     Possible sources of error are readily checked,
    since filtrates can be tested for completeness of
    precipitation and precipitates may be examined for
    the presence of impurities.
     It is an absolute method, i.e. one involving direct
    measurement without any form of calibration being
    required.
     Relatively inexpensive
    GA: Disadvantages

     Time-consuming
     Any interferrents must be removed prior to
    precipitation
     Method is not very sensitive; Only suitable for high
    concentrations
     Applicable to Limited group of elemental analysis
     Volatilisation: Water eliminated in a quantitative
    manner from many inorganic substances by ignition
    is an example of a direct determination. It is
    collected on a solid desiccant and its mass
    determined by the gain in mass of the desiccant
     Determination of the amount of water by measuring
    the loss in mass of the sample during heating is an
    example of an indirect method. (Water of
    crystallization)
    Exercise

     When an sample of impure potassium chloride


    (0.4500g) was dissolved in water and treated with an
    excess of silver nitrate, 0.8402 g of silver chloride
    was precipitated. Calculate the percentage KCl in
    the original sample.
     MW of AgCl = 143.32
     MW of KCl = 74.55

     Ans: 97.12%
    Example

     A mixture of mercurous chloride (FW 472.09) and


    mercurous bromide (FW 560.99) weighs 2.00 g. The
    mixture is quantitatively reduced to mercury metal (At wt
    200.59) which weighs 1.50 g. Calculate the % mercurous
    chloride and mercurous bromide in the original mixture. •
    ANS: 0.5182 g

     1.50 = 2 * 200.59 * x + 2 * 200.59( 2 − x )


    472.09 560.99

     Rearranging and solving:


     0.8498 + 0.7151 2( ) − x = 1.50 x = 0.5182g

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