heavy metals analysis

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    Envirotech Center for Research & Development

    New Delhi

    Harsh K. Dixit

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    NAAQM Standards

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    The Atomic Absorption Spectroscopy technique makes

    use of absorption spectrometry to assess the

    concentration of an analyte in the sample. Method is based on:

    Active sampling using PM10 Respirable Dust Sampler

    & then

    Sample digestion

    Analsis by Atomic absorption spectrophotometer

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    PM10 Sampler

    Hot plate

    Analytical Balance

    Digestion Chamber

    Polypropylene bottle

    GlasswaresAtomic absorption spectrophotometer

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    Filter Paper: 8x10 EPM2000

    Hydrochloric Acid (HCl) concentrated

    Nitric Acid (HNO3) concentratedSulphuric Acid (H2SO4) concentrated

    Metal Standard Solutions

    Sodium borohydridePotassium iodide

    Distilled water

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    1. Microwave Digestion

    2. Hot Plate Digestion

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    Cut filter paper in small pieces

    Place these small pieces into a beaker usingplastic forceps

    Cover the filter with extraction solution

    Place beaker on the hot plate for 30 min.

    Dont allow sample to dry

    Remove beaker from hot plate & allow tocool

    Rinse beaker walls & wash with distilledwater

    Filter the extract and make up to 50 ml.

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    A light beam containing the corresponding

    wavelength of the energy required to raise the

    atoms of the analyte from the ground state to theexcited state is directed through the flame or

    furnace. This wavelength is observed by a

    monochromator and a detector that measure the

    amount of light absorbed by the element, hencethe number of atoms in the ground state in the

    flame or furnace. A hollow cathode lamp for the

    element being determined provides a source of

    that metals particular absorption wavelength.

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    I. Flame atomic absorption: for Pb & Ni

    II. Graphite furnace atomic absorption: forLow detection limit of Pb & Ni

    III. Flame-VGA atomic absorption: for As

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    Choose correct hollow cathod lamp

    Align the instrument

    Position the monochromator Select proper monochromator slit width

    Set the light source current

    Ignite the flame Regulate the flow of fuel & oxidant

    Adjust the burner for maximum

    absorption & stability

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    Choose correct hollow cathod lamp

    Place the furnace

    Align the instrument Position the monochromator

    Select proper monochromator slit width

    Set the light source current

    Switch on chiller

    Regulate the flow of fuel & oxidant

    Adjust the burner for maximum absorption &stability

    Clean graphite tube with a firing

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    C = (Ms Mb) x Vs x Fa/V x Ft

    Where,C = concentration, g metal/m3Ms = metal concentration g/mLMb = blank concentration g/mL

    Vs = total volume of extraction in mLFa = total area of exposed filter in cm2

    V = Volume of air sampled in m3

    Ft = Area of filter taken for digestion in cm2