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    Quantitative Analysis CH 27 Gravimetric Analysis: Gravi - Metric (Weighing - Measure)

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    Namara Temesgen
    Gravimetric analysis is a classical quantitative chemical analysis technique based on determining the mass of a substance that is chemically related to the analyte. There are two main methods: (1) precipitation, where the analyte is converted to an insoluble precipitate, and (2) volatilization, where the analyte is volatilized. Key steps include dissolving the sample, adding excess precipitating reagent, filtering and washing the precipitate, drying, and weighing to determine the analyte content based on the precipitate mass and a gravimetric factor. The goal is to form large, crystalline precipitates that are easily filtered.

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    Quantitative Analysis CH 27 Gravimetric Analysis: Gravi - Metric (Weighing - Measure)

    Uploaded by

    Namara Temesgen
    38 views5 pages
    Gravimetric analysis is a classical quantitative chemical analysis technique based on determining the mass of a substance that is chemically related to the analyte. There are two main methods: (1) precipitation, where the analyte is converted to an insoluble precipitate, and (2) volatilization, where the analyte is volatilized. Key steps include dissolving the sample, adding excess precipitating reagent, filtering and washing the precipitate, drying, and weighing to determine the analyte content based on the precipitate mass and a gravimetric factor. The goal is to form large, crystalline precipitates that are easily filtered.

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    Gravimetric analysis is a classical quantitative chemical analysis technique based on determining the mass of a substance that is chemically related to the analyte. There are two main methods: (1) precipitation, where the analyte is converted to an insoluble precipitate, and (2) volatilization, where the analyte is volatilized. Key steps include dissolving the sample, adding excess precipitating reagent, filtering and washing the precipitate, drying, and weighing to determine the analyte content based on the precipitate mass and a gravimetric factor. The goal is to form large, crystalline precipitates that are easily filtered.

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    38 views5 pages

    Quantitative Analysis CH 27 Gravimetric Analysis: Gravi - Metric (Weighing - Measure)

    Uploaded by

    Namara Temesgen
    Gravimetric analysis is a classical quantitative chemical analysis technique based on determining the mass of a substance that is chemically related to the analyte. There are two main methods: (1) precipitation, where the analyte is converted to an insoluble precipitate, and (2) volatilization, where the analyte is volatilized. Key steps include dissolving the sample, adding excess precipitating reagent, filtering and washing the precipitate, drying, and weighing to determine the analyte content based on the precipitate mass and a gravimetric factor. The goal is to form large, crystalline precipitates that are easily filtered.

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    Quantitative Analysis Ch 27 Gravimetric Analysis

    Classical gravi – metric


    • Gravimetric – mass of analyte (weighing - measure)
    • volumetric (or titrimetric) – volume of solution
    containing sufficient reagent to react completely with
    analyte Chemical analysis based on the determination of
    Instrumental weight of a substance of known composition (the final
    • Electroanalytical – properties resulting from Ox./Red. product) that is chemically related to the analyte.
    behavior of analyte
    • Spectroscopic – measures electromagnetic radiation
    absorbed or emitted by analyte
    • Chromatographic – separates a mixture into its
    components
    1 2

    Gravimetric Analysis Precipitation Method


    • precipitation method: Dissolved analyte (1) The desired substance: completely precipitated.
    converted to sparingly soluble precipitate "common ion" effect can be utilized:
    Ag+ + Cl- à AgCl(s) Ag+ + Cl- AgCl(s)
    excess of Cl- which is added
    • volatilization method: Analyte is volatilized at
    suitable temperature; the volatile product is (2) The weighed form: known composition.
    collected and weighted
    NaHCO3(aq)+H2SO4(aq)àCO2(g)+H2 O(l)+NaHSO4(aq) (3) The product: "pure", easily filtered.
    CO2(g)+2NaOH(s)àNa2CO3(s)+H2 O(l)
    3 4

    avoid colloidal suspension, ideally,


    Steps in Gravimetric Analysis Filtration produce crystals

    (precipitation)
    1) Dry and weigh sample
    2) Dissolve sample
    3) Add precipitating reagent in excess
    4) Coagulate precipitate usually by heating & wait for
    some time (Aging)
    5) Filtration-separate precipitate from mother liquor
    6) Wash precipitate Mother liquor
    7) Dry and weigh to constant weight (0.2-0.3 mg)
    5 6

    1
    Particle Size & Filterability - Precipitates Mechanisms of Precipitation
    Colloids – (d = 10-6 to 10 -4 mm) Two competing processes:
    -invisible to naked eye (1) Nucleation
    -don’t settle out of solution When a small number of
    -difficult or impossible to filter ions, atoms, molecules
    initially unite.
    Particles – (d = 0.10 mm or greater)
    -spontaneously settle out of solution (2) Particle growth
    -readily filtered and washed free of impurities The 3-D growth of a
    -more desirable (typically of higher purity than particle nucleus into a
    colloids) 7
    larger crystal 8

    Particle Size & Filterability - Control Particle Size & Filterability - Control
    Relative supersaturation (RSS)
    RSS = (Q-S)/Q

    Where Q = concentration of solute; S =


    equilibrium solubility of solute

    RSS can be used estimate/control the type of


    precipitate that is formed:
    large: nucleation, small particles (colloids)
    small: particle growth, crystalline solid likely
    9 10

    Techniques to promote crystal growth


    Particle Size & Filterability - Control
    (1) Raising the temperature (increase S).
    The goal is to form crystalline precipitates so RSS
    must be minimized.
    (2) Adding precipitant slowly with vigorous
    mixing (decrease Q).
    Recall:
    RSS = (Q-S)/Q = 1-S/Q (3) Keeping the volume of solution large
    Q = [solute] (decrease Q).
    S = solute’s Equil. Sol.
    This can be done by:
    Increasing S
    Decreasing Q
    11 12

    2
    Treatment of colloidal Precipitates
    pH control of precipitation
    (1) Increasing the electrolyte concentration
    Ca2+ + C2O42- D CaC2O4 (s) •Decreasing the vol. of the counter-ion
    H2C2O4 D 2 H + + C2O42- layer
    •Increasing the chance for coagulation
    Homogeneous Precipitation
    Colloidal Particle of AgCl
    The precipitant is generated slowly by a chemical
    reaction.
    Fe3+ + 3 HCO2- D Fe(HCO2)3⋅nH2O(s)
    HCOOH+OH- D HCO2-+H2O Boundary of ionic
    atmosphere
    (NH2)CO + 3 H2O + heat D OH- + CO2(g)+ 2NH4+
    13 14

    Treatment of colloidal Precipitates


    Treatment of colloidal Precipitates
    (2) Using a volatile electrolyte
    (3) Digestion and aging
    Avoid peptization
    Ex. AgCl, wash with HCl. Drying precipitate at Digestion: Heating the solution for about an hour after
    precipirate formation. This helps to remove weakly
    110°C will remove HCl. bound water
    This displace the less volatile, excess counter ion. Aging: Storing the solution, unheated, overnight. This
    allows trapped contaminates time to “work their way
    out”.
    Both can result in a denser precipitate that is easier to
    filter.

    15 16

    Representative Gravimetric Analyses

    17 18

    3
    Advantages/Disadvantages
    • Experimentally simple and elegant
    • Accurate
    • Precise (0.1-0.3 %)
    • Macroscopic technique-requires at least
    10 mg ppt to collect and weigh properly
    • Time-consuming (1/2 day?)
    19 20

    Calculation Calculation
    • Design of experiment • % of analyte, % A
    • Content Calculation
    • Evaluation of the results
    • %A = weight of analyte x 100
    weight of sample

    • weight of ppt directly obtained à%A


    21 22

    Gravimetric Factor
    How Do We Get %A from ppt?
    • G.F. = a (FW of analyte)
    • % A = weight of ppt x gravimetric factor (G.F.) x 100 b (FW of precipitate)
    weight of sample

    G.F. = a (FW of analyte) • Analyte ppt G.F.


    b (FW of precipitate) CaO CaCO3
    FeS BaSO4
    • G.F. = # gms of analyte per 1 gm ppt UO2(NO3)2.6H2O U3O8
    Cr2O3 Ag2CrO4

    23 24

    4
    Gravimetric Factor Exercise
    • Analyte ppt G.F. • Consider a 1.0000 g sample containing 75%
    CaO CaCO3 CaO/CaCO3 potassium sulfate (FW 174.25) and 25%
    FeS BaSO4 FeS/BaSO4 MSO4. The sample is dissolved and the
    UO2(NO3)2 U3O8 3UO2(NO3)2/U3O8 sulfate is precipitated as BaSO4 (FW
    Cr2O3 Ag2CrO4 Cr2O3/2Ag2CrO4 233.39). If the BaSO4 ppt weighs 1.4900 g,
    what is the atomic weight of M 2+ in MSO4?
    • ANS: Mg2+

    25 26

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