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    Gravimetry

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    CHRISTINE JOY RETARDO
    Gravimetry encompasses techniques that measure mass or changes in mass. Two common gravimetric methods are precipitation gravimetry, where the analyte is separated as a precipitate, and volatilization gravimetry, where the analyte is separated by conversion to a gas. Precipitation gravimetry involves converting the analyte to a soluble precipitate, filtering, washing, and weighing it. The endpoint of a precipitation titration can be determined using a colored ion, colored precipitate, or colored adsorption product as an indicator. Coprecipitation is when other soluble compounds are also removed during precipitation of the analyte.

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    Gravimetry

    Uploaded by

    CHRISTINE JOY RETARDO
    6 views5 pages
    Gravimetry encompasses techniques that measure mass or changes in mass. Two common gravimetric methods are precipitation gravimetry, where the analyte is separated as a precipitate, and volatilization gravimetry, where the analyte is separated by conversion to a gas. Precipitation gravimetry involves converting the analyte to a soluble precipitate, filtering, washing, and weighing it. The endpoint of a precipitation titration can be determined using a colored ion, colored precipitate, or colored adsorption product as an indicator. Coprecipitation is when other soluble compounds are also removed during precipitation of the analyte.

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    Analytical Chemistry (Qualitative and Quantitative Chemistry)

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    Gravimetry encompasses techniques that measure mass or changes in mass. Two common gravimetric methods are precipitation gravimetry, where the analyte is separated as a precipitate, and volatilization gravimetry, where the analyte is separated by conversion to a gas. Precipitation gravimetry involves converting the analyte to a soluble precipitate, filtering, washing, and weighing it. The endpoint of a precipitation titration can be determined using a colored ion, colored precipitate, or colored adsorption product as an indicator. Coprecipitation is when other soluble compounds are also removed during precipitation of the analyte.

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    © All Rights Reserved
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    Download as pdf or txt
    6 views5 pages

    Gravimetry

    Uploaded by

    CHRISTINE JOY RETARDO
    Gravimetry encompasses techniques that measure mass or changes in mass. Two common gravimetric methods are precipitation gravimetry, where the analyte is separated as a precipitate, and volatilization gravimetry, where the analyte is separated by conversion to a gas. Precipitation gravimetry involves converting the analyte to a soluble precipitate, filtering, washing, and weighing it. The endpoint of a precipitation titration can be determined using a colored ion, colored precipitate, or colored adsorption product as an indicator. Coprecipitation is when other soluble compounds are also removed during precipitation of the analyte.

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    © All Rights Reserved
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    of 5

    GRAVIMETRY

    GRAVIMETRY
    ★ Gravimetry encompasses all techniques in which we measure mass or a change in mass. When you step on a scale after
    exercising you are making, in a sense, a gravimetric determination of your mass. Measuring mass is the most
    fundamental of all analytical measurements, and gravimetry is unquestionably the oldest analytical technique.

    Two methods of gravimetry:


    A. Precipitation Gravimetry
    - The analyte is separated from a solution of the sample as a precipitate and is concentrated to a
    compound of known composition that can be weight
    B. Volatilization gravimetry
    - The analyte is separated from other constituents of a sample by conversion to a gas of known chemical
    composition.

    Other types of gravimetric methods:


    ➔ Electrogravimetry - The analyte is separated by a deposition on an electrode by an electrical current.
    ➔ Gravimetric Titrimetry - The mass of a reagent of known concentration is required to react completely with
    the analyte provides the information needed to determine the analyte concentration.
    ➔ Atomic mass Spectrometry - Uses a mass spectrometer to separate the gaseous ions formed from the
    elements making up a sample matter.

    PRECIPITATION GRAVIMETRY

    ★ The analyte is converted to soluble precipitate. This precipitate is then filtered, washed free of impurities converted
    to a product of known composition by suitable heat treatment and weight.
    ★ Example:

    DOUBLE DISPLACEMENT

    ★ A double displacement reaction is a type of reaction in which two reactants exchange ions to form two new
    compounds. Double displacement reactions typically result in the formation of a product that is a precipitate.
    ★ A double displacement reaction is a type of chemical reaction in which the reactant ions exchange places to form
    new products.
    ★ Usually, a double displacement reaction results in precipitate formation.
    ★ The chemical bonds between the reactants may be either covalent or ionic.
    ★ A double displacement reaction is also called a double replacement reaction, salt metathesis reaction, or double
    decomposition.
    PRECIPITATION REACTION

    Properties of precipitates and precipitating agents:


    ➔ Ideally a gravimetric precipitating agent should react SPECIFICALLY or at least SELECTIVELY with the analyte.
    A. Specific Reagents - React only with the single chemical species. (RARE)
    B. Selective Reagents - react with a limited number of species. (MORE COMMON)
    C. Precipitant/precipitating agent
    ➔ Ideally the reagents would react with the analyte to give a product that is:
    1. easily filtered and washed free of contaminants;
    2. of sufficiently low solubility that no significant loss of the analyte occurs during filtration and washing;
    3. unreactive with constituents of the atmosphere;
    4. of known chemical composition after it is dried or, if necessary, ignited.

    Particle size and filterability of precipitates


    ➔ Colloidal Suspensions - solids are tiny particles that are invisible to the naked eye. These particles show no tendency
    to settle from the solution and are not easily filtered.
    ➔ Crystalline Suspension - particles tend to settle spontaneously and are easily filtered.
    ➔ Particle size of ppt. is influenced by experimental variables such as:
    1. Precipitate Solubility
    2. Temperature
    3. Reactant Concentration
    4. Rate at which reactants are mixed.

    COLLOIDAL PRECIPITATE

    ★ Particles in the colloidal precipitates are so small that they are not retained by ordinary filters. Brownian motion
    prevents their settling out of solution under the influence of gravity. Coagulate or agglomerate the particles to form a
    filterable amorphous mass that will settle out of solution.
    ★ Coagulation of Colloids - Coagulation can be hastened by heating, stirring and by adding an electrolyte to the medium.
    Colloidal particles are stable due to positively or negatively charged particles.
    ★ Peptization of Colloids - Peptization is the process by which a coagulated colloid reverts its original dispersed state.
    When a coagulated colloid is washed some of the electrolytes responsible for its coagulation is leached from the internal
    liquid in contact with the solid particles.
    Peptization Coagulation

    Peptization is the process in which a precipitate is In the coagulation process, the colloids get destabilized and
    converted into a colloidal solution. This is done by they change into larger sizes particles ultimately settling as
    shaking it properly with an electrolyte. a precipitate.

    The electrolyte which is added to it generally has one The electrolyte added for coagulation process generally has
    common ion with the precipitate. one oppositely charged ion to the one in the sol.

    The suitably charged ions are adsorbed by the precipitate The electrical charge of the particles in the dispersed phase
    particles giving it either a negative or positive charge. The gets neutralized and this results in the colloidal particles
    like-charged particles repel each other and break the getting aggregated.
    precipitate into smaller particles of the size of colloid
    particles.

    An example of peptization: An example of coagulation:

    Addition of ferric chloride into freshly prepared ferric Addition of aluminum chloride into negatively charged sol
    hydroxide As2S3

    FCl3 -> Fe3+ + 3Cl-

    Fe(OH)3 + Fe3+ → [Fe(OH)3]Fe3+

    Coprecipitation Post Precipitation

    Definition Coprecipitation is a type of precipitation Post precipitation is a type of precipitation


    where soluble compounds in a solution where the precipitation of undesirable
    are removed during the course of compounds occurs after the formation of the
    precipitation precipitate of the desirable compound

    Degree of contamination High Low

    Time of precipitation During the desirable precipitation After the desirable precipitation

    Examples Precipitation of silver ions with other Formation of calcium oxalate after the
    silver chloride precipitation precipitation of magnesium oxalate
    COPRECIPITATION

    ★ is a phenomenon in which otherwise soluble compounds are removed from the solution during precipitate formation.

    There are four types of coprecipitation


    1. Surface Adsorption
    2. Mixed Crystal formation
    3. Occlusion
    4. Mechanical entrapment

    REPRECIPITATION

    ★ Drastic but effective way to minimize the effects of adsorption.


    ★ The filtered solid is redissolved and reprecipitated. The first ppt. ordinarily carries down only a fraction of the
    contaminant present in the original solution.
    Precipitation from homogeneous solution.
    • Precipitation from homogeneous solutions is a technique in which a ppt agent is generated in a solution of the
    analyte by a slow chemical reaction.

    PRECIPITATION METHOD

    ★ Is also known as ARGENTOMETRIC ANALYSIS


    ★ Analyte is titrated with a standard solution of a precipitating agent in the presence of an appropriate indicator.
    ★ It applies the solubility product principle, which states that in a saturated solution of an ionic compound, the product of
    the molar activities has a constant value at any particular temperature and pressure.
    ★ Ionic product exceeds the Ksp value (Solubility product constant) of the compound – precipitation will proceed

    ENDPOINT
    ★ The endpoint is determined by
    - Formation of precipitate
    - Appearance of turbidity
    - Instrumental methods
    - Internal indicators
    ➔ COLORED ION – VOLHARD METHOD
    ➔ COLORED PRECIPITATE – MOHR METHOD
    ➔ COLORED ADSORPTION PRODUCT – FAJAN METHOD

    COLORED ION (VOLHARD METHOD)


    ★ JACOB VOLHARD
    ★ Titrant/VS/Standard Solution = Ammonium thiocyanate (NH4SCN)
    ★ Indicator = Ferric Alum or FAS (Ferric Ammonium Sulfate)
    ★ Secondary precipitate = Ferric thiocyanate Fe(SCN)3
    ★ Endpoint = Reddish brown color

    COLORED SECONDARY PRECIPITATE (MOHR METHOD)


    ★ KARL FRIEDRICH MOHR
    ★ Titrant/VS/Standard Solution = Silver Nitrate
    ★ Indicator = Potassium chromate (K2CrO4)
    ★ Secondary precipitate = Silver chromate
    ★ Endpoint = White to Reddish colored mixture

    COLORED ADSORPTION PRODUCT (FAJAN METHOD)


    ★ KAZIMIERZ FAJAN
    ★ Titrant/VS/Standard Solution = Silver Nitrate
    ★ Indicator = DCF, TEE, Eosin Y
    ★ Endpoint = Yellowish green to reddish pink

    GRAM EQUIVALENT WEIGHT - The gram eq wt. of a substance in the precipitation method is obtained by dividing the
    molecular weight by the total valence of the precipitating or precipitated ion.

    COMPOUNDS ASSAYED
    - Determination of Halogens
    - Thiocyanate
    - Cyanide

    STANDARD SOLUTIONS
    ❑SILVER NITRATE - a colorless crystalline solid becoming black on exposure to light. A silver salt with powerful germicidal
    activity. It can potentially be used as cauterizing or sclerosing agent.
    ❑AMMONIUM THIOCYANATE – a colorless crystalline solid. It is soluble in water. It is used in chemical analysis, in
    photography, as a fertilize, and other uses.
    ❑POTASSIUM THIOCYANATE – an important salt of the thiocyanate anion. The compound has a low melting point relative
    to most inorganic salts.

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