Gravimetric Analysis Ppt Chem

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    Weighing the sample Forming a precipitate Filtering the solution Weighing the dry precipitate

    This analytical technique includes: Empirical formula and Molecular formula

    Gas equations Eg. Pv=nrt

    Percentage of water/ measuring water content

    Limiting and Excess reactant equations

    Precipitation reactions

    Key steps in a

    precipitation reaction-

    what this looks like

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    #1: Accurately weigh the

    mixture to be analysed.

    #4: Filter off the precipitate

    and wash it with a small

    quantity of substance.

    #2: Dissolve the mixture in a

    suitable solvent; filter off anddiscard any insoluble material.

    #3: Add an excess amount of

    solution, that will form a

    precipitate with the substance

    being analysed.

    #5: Dry the precipitate and,

    cool and accurately weigh.Repeat until a constant mass is

    achieved.

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    Gravimetric analysis is a technique through which the

    amount of an analyte (the ion being analyzed) can be

    determined through the measurement of mass.

    Gravimetric analysis depend on comparing the masses of

    two compounds containing the analyte.

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    Advantages

    Precise measurement/

    high degree of accuracy

    (6-figure)

    Helps in determination ofatomic mass, of elements

    Doesnt require a series of

    standards to calibrate the

    unknown solution

    concentration Helps in calibration of

    other instruments

    Disadvantages

    Limited group of

    elemental analysis

    Convoluted methods

    Only suitable for highconcentrations

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    Gravimetric analytical data is interpreted from the

    weighing of the precipitate at the end of the experiment.

    To do this, you must weigh the instrument in which the

    precipitate will be weighed in, note the weight, and then

    weigh the precipitate. The solid weight is determined bythe difference between the two.

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    Calibration is predominantly undertaken by gravimetricanalysis and is the method most commonly used bylaboratories accredited to ISO17025. There are colorimetricmethods in use and these are often used for checking pipettesand for non-accredited calibration. Gravimetric analysis ispreferred due to the simplicity and the traceability to an

    absolute standard. Gravimetric methods are also oftenrecognsied as a more economical way of calibration.

    Gravimetric analysis for pipette calibration entails dispensingsamples of distilled water into a receiving vessel in aprecision analytical balance. The density of water is a known

    constant, the temperature, barometric pressure and humidityare recorded (the Z-factor used in the final mass calculation)and kept within certain limits and thus the mass of thedispensed sample provides an accurate indication of thevolume dispensed.

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    Determination of atomic

    mass of elements

    Purity evaluation

    Determining water content of

    complex materials. Eg. Food

    and soil

    Treating ore (part

    of earths layer)

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    Geomarine survey systems

    A chunk of ore is treated with concentrated nitric acid and

    potassium chlorate to convert all of the sulfur to sulfate.

    The nitrate and chlorate are removed by treating the

    solution with concentrated HCl. The sulfate is precipitatedwith Barium and weighed as BaSo4.

    Monitoring the air

    Sulfate with

    nitrate and

    chlorate

    Concentrated HCl to

    remove nitrate and

    chlorate BaSO4

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    Gravimetric analysis obtains more accurate data about the

    composition of a sample than volumetric analysis does,

    however it takes longer to perform in the laboratory.

    Gravimetric analysis is analysis by weight, where as

    volumetric analysis is by volume. Gravimetric analysis is less sensitive to temperature than

    volumetric analysis is.

    volumetricGravimetric-less sensitive

    Temp.

    Gravimetric-weight

    Volumetric- volume

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    Looks like a titration/ same as

    Measure from bottom of meniscus

    Wherever there is a concentration of a known solution, to

    be found, then volumetric analysis is the method to use.

    Quantative analytical technique

    Measure from bottom

    of meniscus

    Titration/

    volumetric

    analysis

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    Steps

    Clean the pipette and rinse it with a

    bit of the solution to be used.

    Clean a conical flask using distilled

    water.

    Pipette the specified volume of one

    reactant into the flask.

    Rinse down the edges of the flaskwith distilled water.

    Add the indicator if required.

    Clean the burette and rinse with bit

    of the second reactant solution. Fill

    with the solution. Does not need to

    be exactly on zero. Note the reading

    on the bottom of the meniscus.

    Perform a preliminary (rough)

    titration by running the burette

    solution into the flask, making sure to

    swirl the mix, until the end point is

    reached.

    Read the meniscus again. Subtract the

    first reading to find the volume

    added.

    Repeat the first 5 steps.

    Read the burette and perform an

    accurate titration by repeating step

    7.

    Stop as soon as the end point is

    reached.

    Subtract the initial reading from theend point reading to give an accurate

    titre.

    Repeat the accurate titration (steps

    9-12) at least twice more. The titres

    should be within 0.1cm of each other.

    Take an average of your three

    accurate titres. Use this as the

    volume added in the calculations.

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    Equipment

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    Advantages

    Fast and easy to perform

    Only basic laboratory

    equipment needed

    Very cheap Accurate results

    Different methods

    available for different

    substances

    Disadvantages

    Relatively large sample

    size needed

    Only suitable for relatively

    high concentrations

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    Data is interpreted by using three concordant titres. These

    help to give accurate results and need to be within 0.1 of

    each other.

    Concordant titres- they shouldall be a similar colour

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    To ensure proper measurement of

    large volumes in the laboratory,

    volumetric apparatus should be

    calibrated regularly. Two of the most

    common apparatus calibrated are

    volumetric flasks and serological

    pipettes.

    *If the error is more than 0.03% then

    the apparatus should be discarded or

    changed into a volumetric apparatus

    Manual procedure via volumetric flask

    - Weigh the volumetric flask.

    - Fill the volumetric flask with distilled

    water, up to the mark

    - Weigh the volume of distilled water

    contained in the flask.

    - Calculate the true volume of

    glassware via the formula

    - Record the data

    - Do the same procedure with the

    serological pipette.

    - Record again your data.

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    Used in bio diesel manufacture to ensure that the mix has

    a neutral pH.

    To determine the amount of acetic acid in manufactured

    vinegar.

    To determine fatty-acid content and unsaturated-fatty acidcontent.

    Brain imaging and MR imaging, as well as routine clinical

    use.

    Suitable for direct titrations

    Suitable in Determination of iron

    Manufactured

    vinegar

    brain imaging

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    Compared to other analysis; for example gravimetric

    analysis, volumetric analysis is less accurate and less

    reliable.

    In volumetric analysis, you are more likely to encounter

    limits of sensitivity in volume measurements, compared toother analytical techniques.

    A mass is generally easier to determine and standardize

    than a concentration.

    Errors associated with volume measurements are

    minimized in other analytical techniques, such asgravimetric analysis.

    Volumetric analysis less accurate