heavy metals analysis
TRANSCRIPT
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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